CN105067470B - A kind of surface reaction detection device and its method for detection - Google Patents
A kind of surface reaction detection device and its method for detection Download PDFInfo
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Abstract
The present invention provides a kind of surface reaction detection device and its detection method.Surface reaction detection device includes vacuum atmosphere furnace system, mass measurement system and electromagnetic rotating system, pass through the driving effect of electromagnetic rotating system, drive the loading rotor horizontal rotation of mass measurement system to overcome and the defect that tested sample must be static is required in existing thermogravimetric technology, by existing thermogravimetric technique improvement into a kind of dynamic thermogravimetric technology that the sample of inner ring carbon outer shroud titanium dioxide can be made to carry out controllable spinning campaign in chlorine atmosphere, to realize dynamic measurement.The detection method provided using the present invention can be under the influence of centrifugal force, the mass loss Δ m of sample in the unit interval is measured using the DTG, and then calculate reaction rate to judge to react the surface that intermediate medium material is preferentially formed, the forming feature for the further intermediate medium of research titanium oxide carburizing chlorination reaction provides important evidence.
Description
Technical field
The invention belongs to surface reaction process detection technique field, and in particular to a kind of surface reaction detection device and its detection
Method.
Background technology
It can be seen from the oxygen gesture figure of metal oxide and chlorine gesture figure, titanium oxide, particularly titanium dioxide are can not be direct
Chloride is changed into by the chlorination of chlorine institute.But in the presence of having the reducing agents such as carbon, become the chlorination of titanium dioxide
For may, and the reactivity worth of itself and chlorine significantly increases.Carburizing chlorination reaction is that a gas phase and two are solid
Phase --- TiO2, C participate in complicated heterogeneous reaction.Domestic and international experts and scholars have carried out numerous studies to it, successively propose
Many viewpoints for explaining this macroscopic appearance, a class viewpoint thinks TiO2It is reduced to first by C after titanium suboxide again by chlorine
It is melted into TiCl4.However, under the conditions of actual chlorination furnace reaction temperature, the probability that C direct-reduction effect is produced is little, TiO2Quilt
The speed that carbon is reduced to titanium suboxide is very low, it is impossible to explain the fact that carburizing chlorination reaction rate is significantly improved.Separately
One class viewpoint thinks there is the intermediate product i.e. presence of intermediate medium, although TiO2With Cl2The standard free enthalpy of reaction be on the occasion of, but
Still minimal amount of TiCl is had in reaction system4Produce, exactly this minimal amount of TiCl4Absorption is in TiO2In Surface Creation
Between product further with C and Cl2React and form final product TiCl4；In addition, being additionally considered that the reducing agent C and O of addition2Instead
The partial pressure of oxygen of chlorination formation should be able to be reduced, solid carbon is changed into CO, and Cl2With CO reaction generations COCl or COCl2Deng intermediate product
Afterwards, then with TiO2Generation chlorination reaction formation product TiCl4。
In a word, above-mentioned viewpoint is all based on explanation and supposition of the thermodynamic analysis to macroscopic appearance, and its key point is to determine
Cl2、TiO2The intermediate medium for promoting this reaction of reaction sequence and generation between C three.Therefore exploitation can detect surface
The instrument and experimental method of reaction rate, react, tool is of great significance for studying such surface.
The content of the invention
For deficiencies of the prior art, the invention provides a kind of surface reaction detection device and its side of detection
Method, can make to cause intermediate medium can in different in nature turn into carbon particle surface and titanium oxide adsorption Low Response by the present invention
The reaction process of control, to reach that research titanium oxide carburizing chlorination reacts the formation of intermediate medium and the purpose of pipeline.
To achieve these goals, the technical solution adopted by the present invention is as follows：
A kind of surface reaction detection device, including vacuum atmosphere furnace system, mass measurement system and electromagnetic rotating system；It is described
Vacuum atmosphere furnace system include boiler tube, furnace shell and heating mantle；Described furnace shell is in integrally the casing of inner hollow, and described adds
Hot jacket is enclosed on outside furnace shell, for giving the heating of vacuum atmosphere furnace system；Described furnace shell top is provided with blast pipe；Described stove
Mounting hole is also provided with the top of shell, for being socketed described boiler tube；Described boiler tube is that the entirety being vertically arranged is closed in upper surface
Lower surface is open tubular, and the boiler tube is fastened in furnace shell, and space is left between the opening and the inner bottom surface of furnace shell of tubular,
Described boiler tube and the inner space of furnace shell constitute the confined space that can be evacuated；The center of the top surface of described boiler tube
It is provided with the connecting hole for quality of connection measuring system；Described boiler tube top is connected with air inlet pipe I and air inlet pipe II, it is described enter
Tracheae I and air inlet pipe II extend to inside the boiler tube and the mouth of pipe straight down；Described mass measurement system is passed including quality
Sensor, suspension wire, inverted U-shaped suspension ring, bearing connector, connecting rod and load sample rotor；The mass sensor can detect suspension
The change of material mass and quality thereunder；Described suspension wire is vertically arranged, and its upper end is fixed with mass sensor
Connection, lower end and the peak of inverted U-shaped suspension ring are removably joined together, and described bearing connector is fixed on the U
In two ring arm of shape suspension ring；Described connecting rod is vertically arranged, and its upper end is rotationally connected with bearing connector, can be in connecting rod
Keep inverted U-shaped suspension ring static when horizontally rotating, described connecting rod extends to the stove by the connecting hole positioned at boiler tube top surface center
In pipe, the lower end of described connecting rod is fixed on the central point of the loading rotor；The loading rotor is horizontally disposed entirety
Shape axisymmetricly, can be under the driving of electromagnetic rotating system using the central point of loading rotor as pivot level turn
It is dynamic；Described electromagnetic rotating system is arranged on the lower section of described furnace shell bottom, including motor and driving rotor；The driving of motor
Axle is vertically arranged, and can be horizontally rotated under the driving of motor, and the top of the drive shaft is fixed on the center of the driving rotor
Point, the driving rotor is the shape of horizontally disposed entirety axisymmetricly, can be driven under the driving of motor in rotor
Heart point horizontally rotates for pivot, and drives loading rotor to rotate in the presence of magnetic force induction.
Further, described boiler tube is in the dumb-bell shape being vertically arranged, and inside is a dumb-bell shape cavity, and the bottom of boiler tube is spacious
Mouthful, dumb-bell shape cavity to be connected with furnace shell inner space.
Further, described bearing connector is made up of horizontally disposed bearing I and bearing II, described bearing I and axle
II line of centres and the central axis of connecting rod are held on a plumb line, connecting rod can be made not shifted when horizontally rotating
With rock.
Further, described connecting rod be upper and lower two sections, two sections between be removably joined together；Described boiler tube top
Face is provided with a dress sample hole, and dress sample hole overlying has the closure for closing the boiler tube, and the closure is detachably connected to
The top surface of the boiler tube.
Further, described load sample rotor and the correspondence position in sample gap are provided with the perpendicular of several equidistant diameter 1mm
To through hole.
Further, check valve is provided with described blast pipe, the check valve is only capable of beating to the side opposite with furnace shell
Open.
Further, the range of described mass sensor is 0~300g, and accuracy is 0.5mg.
Further, Resistant heating body of the described heating mantle inside body and body is constituted.
A kind of sample used cooperatively with above-mentioned surface reaction detection device, including two pieces of annular coupons I, coupons II
With some platinum pieces；The internal diameter of described coupon I is identical with the external diameter of described connecting rod, and the internal diameter of described coupon II is big
In the external diameter of coupon I, the diameter of coupon II is less than the length of described loading rotor；Described coupon I is placed on examination
In the ring of sample block II, platinum piece is stuck between coupon I and coupon II.
A kind of method for detecting the reaction of titanium dioxide carburizing chlorination, this method uses above-mentioned surface reaction detection device, its
Step includes：
1）Sample preparation：The sample of claim 9 is made, wherein coupon I is made up of carbon, and coupon II is by titanium dioxide system
Into；
2）Be powered preheating：Heating mantle is opened to heat vacuum atmosphere furnace system, by the way of gradually heating up, heating
Preheated to 900 DEG C, preheating time is not less than 30 minutes；
3）Fill sample：Coupon I on sample is enclosed on connecting rod and fallen on loading rotor, boiler tube is then slowly put into
It is interior, in-furnace temperature is risen into 1000 DEG C of reaction temperature, and keep constant；
4）Ventilation：First the air in the confined space of vacuum atmosphere furnace system is evacuated down to by described blast pipe-
0.097MPa；Air inlet pipe II is connected into argon bottle again, argon gas is injected into boiler tube with 2L/min flow；
The initial mass m of sample is measured and recorded by mass sensor1, then air inlet pipe I connected into chlorine cylinder, with 2L/
Min flow injects chlorine into boiler tube, carries out chlorination reaction；Record the mass change Δ m in the sample unit interval1, by this
Under the conditions of carburizing chlorination reaction rate be designated as Δ m1/Δt；
5）Speed governing is detected：By the electric motor starting of described electromagnetic rotating system, and regulation motor rotating speed is so that loading rotor
Rotating speed it is constant, record the sample unit interval in mass change Δ m2, the carburizing chlorination under centrifugal forces affect is reacted into speed
Rate is designated as Δ m2/Δt；
6）Shutdown：First close motor, heating mantle and chlorine cylinder, by confined air from air inlet pipe II to vacuum atmosphere furnace system
It is interior to continue logical argon gas, until the quality that mass sensor is detected no longer changes；
7）Interpretation of result：If the carburizing chlorination reaction rate Δ m under having centrifugal action2/ Δ t is more than under inactive state
Carburizing chlorination reaction rate Δ m1During/Δ t, illustrate that intermediate medium is generated in carbon surface；If Δ m2/ Δ t is less than Δ m1During/Δ t,
Illustrate that intermediate medium is generated in titanium dioxide surface.
Compared with prior art, the present invention has the advantages that：
1st, in the presence of by electromagnetic rotating, overcome and the defect that tested sample must be static required in existing thermogravimetric technology,
Existing thermogravimetric technique improvement is carried out into a kind of sample that can make inner ring carbon outer shroud titanium dioxide in chlorine atmosphere controllable
Spinning campaign dynamic thermogravimetric technology.
2nd, under the influence of centrifugal force, mass loss the Δ m, Jin Erji of sample in the unit interval are measured using the DTG
Calculate reaction rate to judge to react the surface that intermediate medium material is preferentially formed, be that further research titanium oxide carburizing chlorination is anti-
The forming feature for the intermediate medium answered provides important evidence.
Brief description of the drawings
Fig. 1 is structural representation of the invention；
Fig. 2 is sample mounting structure sectional view of the invention.
In accompanying drawing：1-mass sensor；2-suspension wire；3-inverted U-shaped suspension ring；4-bearing I；5-air inlet pipe I；6—
Furnace shell；7-heating mantle；8-driving rotor；9-motor；10-load sample rotor；11- samples；12- connecting rods；13- blast pipes；14-
Boiler tube；15- air inlet pipe II；16- bearings II.
Embodiment
The present invention is described in further detail with reference to specific embodiment.
As shown in figure 1, a kind of surface reaction detection device, it is characterised in that including vacuum atmosphere furnace system, mass measurement system
System and electromagnetic rotating system；
Described vacuum atmosphere furnace system includes boiler tube 14, furnace shell 6 and heating mantle 7；Described furnace shell 6 is overall in inside
Empty casing, described heating mantle 7 is enclosed on outside furnace shell 6, for giving the heating of vacuum atmosphere furnace system；The described top of furnace shell 6
It is provided with blast pipe 13；The described top of furnace shell 6 is also provided with mounting hole, for being socketed described boiler tube 14；Described boiler tube 14
In upper surface closed lower face be open tubular for the entirety that is vertically arranged, the boiler tube 14 is fastened in furnace shell 6, tubular it is spacious
Space is left between mouth and the inner bottom surface of furnace shell 6, described boiler tube 14 and the inner space of furnace shell 6, which are constituted, can be pumped into very
Empty confined space；The center of the top surface of described boiler tube is provided with the connecting hole for quality of connection measuring system；Described stove
The top of pipe 14 is connected with air inlet pipe I 5 and air inlet pipe II 15, and the air inlet pipe I 5 and air inlet pipe II 15 are extended in the boiler tube 14
The portion and mouth of pipe is straight down；
Described mass measurement system includes mass sensor 1, suspension wire 2, inverted U-shaped suspension ring 3, bearing connector, company
Bar 12 and load sample rotor 10；The mass sensor 1 can detect the change of the material mass being hung below and quality；Institute
The suspension wire 2 stated is vertically arranged, and its upper end is fixedly connected with mass sensor 1, and the peak of lower end and inverted U-shaped suspension ring 3 can
Releasably link together, described bearing connector is fixed in two ring arm of the inverted U-shaped suspension ring 3；Described connecting rod 12
It is vertically arranged, its upper end is rotationally connected with bearing connector, can keeps inverted U-shaped suspension ring 3 quiet when connecting rod horizontally rotates
Only, described connecting rod 12 is extended in the boiler tube 14 by the connecting hole positioned at the top surface of boiler tube 14 center, described connecting rod 12
Lower end is fixed on the central point of the loading rotor 10；The loading rotor 10 is the shape of horizontally disposed entirety axisymmetricly
Shape, central point that can be using loading rotor 10 under the driving of electromagnetic rotating system horizontally rotates as pivot；
Described electromagnetic rotating system is arranged on the lower section of the described bottom of furnace shell 6, including motor 9 and driving rotor 8；Electricity
The drive shaft of machine 9 is vertically arranged, and can be horizontally rotated under the driving of motor 9, and the top of the drive shaft is fixed on the driving
The central point of rotor 8, the driving rotor 8 be the shape of horizontally disposed entirety axisymmetricly, can under the driving of motor 9 with
The central point of driving rotor 8 horizontally rotates for pivot, and drives loading rotor 10 to rotate in the presence of magnetic force induction.
As a preferred embodiment, described boiler tube 14 is in the dumb-bell shape being vertically arranged, inside is a dumb-bell shape
Cavity, the bottom of boiler tube 14 is opening, dumb-bell shape cavity to be connected with the inner space of furnace shell 6.Boiler tube is designed as this shape
Shape, can make reacting gas and scope that sample meets in boiler tube smaller, so that reaction is more abundant.
As a preferred embodiment, described bearing connector is by II 16 groups of horizontally disposed bearing I 4 and bearing
Into the central axis of the line of centres and connecting rod of bearing I 4 and bearing II 16 can make connecting rod in level on a plumb line
Do not shift and rock during rotation.
As a preferred embodiment, for the ease of sample 11 is sleeved on connecting rod 12, described connecting rod 12 is
It is removably joined together between upper and lower two sections, two sections；Sample 11 is loaded in the case of in order to not remove boiler tube 14, can be
The described top surface of boiler tube 14 opens a dress sample hole, and dress sample hole overlying has the closure for closing the boiler tube, and the closure can
Releasably it is connected to the top surface of the boiler tube.
As a preferred embodiment, in order that chlorine is convenient with being produced after the reaction of sample 11 and discharge reaction in time
Thing, the correspondence position in described load sample rotor 10 Yu the gap of sample 11 is provided with several equidistant diameter 1mm vertical through holes.
As a preferred embodiment, be provided with check valve in described blast pipe 13, the check valve be only capable of to
The side opposite with furnace shell is opened, in order to the gas that the discharge air of orientation and reaction are produced, anti-backflow.
As a preferred embodiment, in order that accuracy of detection meets the requirement of experiment, described mass sensor 1
Range should be selected to be the mass sensitivity equipment that 0~300g, accuracy are 0.5mg.
As a preferred embodiment, Resistant heating body group of the described heating mantle 7 inside body and body
Into.
A kind of sample 11 used cooperatively with above-mentioned surface reaction detection device, it is characterised in that including two pieces of annular examinations
Sample block I, coupon II and some platinum pieces；The examination identical, described with the external diameter of described connecting rod of the internal diameter of described coupon I
The internal diameter of sample block II is more than the external diameter of coupon I, and the diameter of coupon II is less than the length of described loading rotor；Described examination
Sample block I is placed in the ring of coupon II, and platinum piece is stuck between coupon I and coupon II, so that distance therebetween
Keep constant.
A kind of method for detecting the reaction of titanium dioxide carburizing chlorination, it is characterised in that used above-mentioned surface reaction detection
Device and sample 11, its step include：
1）Sample preparation：Coupon I is made in carbon, coupon II is made in titanium dioxide, then platinum piece is stuck in coupon I and examination
Between sample block II, so that distance therebetween keeps constant；
2）Be powered preheating：Open heating mantle 7 to heat vacuum atmosphere furnace system, by the way of gradually heating up, rise
Warm to 900 DEG C are preheated, and preheating time is not less than 30 minutes；
3）Fill sample：By the sample 11 being made insert in connecting rod it is fixed as shown in Fig. 2 and be slowly put into boiler tube 14, by temperature
Degree rises to 1000 DEG C of reaction temperature, and keeps constant；
4）Ventilation：First the air in the confined space of vacuum atmosphere furnace system is vacuumized by described blast pipe 13
To -0.097MPa；Air inlet pipe II 15 is connected into argon bottle again, argon gas is injected into boiler tube 14 with 2L/min flow；
The initial mass m1 of sample 11 is measured and recorded by mass sensor 1, then air inlet pipe I 5 is connected into chlorine cylinder, with
2L/min flow injects chlorine into boiler tube 14, carries out chlorination reaction；Record the mass change Δ in the unit interval of sample 11
m1, carburizing chlorination reaction rate under the conditions of this is designated as Δ m1/Δt；
5）Speed governing is detected：The motor 9 of described electromagnetic rotating system is started, and the rotating speed of regulation motor 9 is so that loading turns
The rotating speed of son 10 is constant, the mass change Δ m in the record unit interval of sample 112, by the carburizing chlorination under centrifugal forces affect
Reaction rate is designated as Δ m2/Δt；
6）Shutdown：First close motor, heating mantle and chlorine cylinder, by confined air from air inlet pipe II to vacuum atmosphere furnace system
It is interior to continue logical argon gas, until the quality that mass sensor is detected no longer changes；
7）Interpretation of result：If the carburizing chlorination reaction rate Δ m under having centrifugal action2/ Δ t is more than under inactive state
Carburizing chlorination reaction rate Δ m1During/Δ t, illustrate that intermediate medium is generated in carbon surface；If Δ m2/ Δ t is less than Δ m1During/Δ t,
Illustrate that intermediate medium is generated in titanium dioxide surface.
, can be with repeat step 5 in order to increase the accuracy of experimental result）Record the matter in the unit interval under different rotating speeds
Measure changes delta m3……ΔmnWith the carburizing chlorination reaction rate Δ m under centrifugal forces affect3/Δt……Δmn/Δt；According to
Mass change Δ m in unit interval1……ΔmnWith the carburizing chlorination reaction rate Δ m under centrifugal forces affect1/Δt……
Δmn/ Δ t analyzes testing result.If the carburizing chlorination reaction rate Δ m under having centrifugal action2/Δt……Δmn/ Δ t is big
In the carburizing chlorination reaction rate Δ m under inactive state1During/Δ t, illustrate that intermediate medium is generated in carbon surface；If Δ m2/Δ
t……Δmn/ Δ t is less than Δ m1During/Δ t, illustrate that intermediate medium is generated in titanium dioxide surface.
The material of sample coupon I and coupon II can be exchanged, and the result of the test inference method after exchange is identical.
The Cleaning Principle of the present invention：Because the mass sensor measurement accuracy of DTG is higher, motor 9 can not be directly with turning
Son is connected, so design motor 9 is connected with driving rotor 8, driving rotor 8 drives loading rotor 10 to rotate by electromagnetic force, and
Realize motor 9 with being indirectly connected with for rotor so that DTG is smoothed out.According to experiment the rotation for adjusting motor can be needed fast
Degree, in the presence of rotary centrifugal force, carbon（C）The intermediary material desorption rate generated on surface is improved, it is easier to reached
Titanium dioxide（TiO2）Surface, it is high when can make reaction rate than not revolving reaction；Conversely, titanium dioxide（TiO2）Surface Creation
Intermediary material desorption is drawn up, low when causing reaction rate than not rotatable reactor.So, it is possible to use DTG is surveyed
The mass loss Δ m for obtaining sample in the unit interval judges reaction rate to judge to react the middle intermediary table of fine quality being initially formed
Face.
It can be seen from carburizing chlorination reaction equation, reaction generation gas TiCl4、CO2And CO, the matter of carbon and titanium dioxide sample
Amount can be gradually decreased with the progress of reaction, and its reaction rate can be according to the mass loss Δ m of sample in the unit interval
Calculating is obtained, plus carbon promotes the essence of titanium dioxide chlorination reaction to be, intermediary is generated therebetween, can be according to experiment need
Adjust the rotary speed of motor, in the presence of rotary centrifugal force, carbon（C）The intermediary material desorption speed generated on surface
Degree is improved, it is easier to reach titanium dioxide（TiO2）Surface, it is high when can make reaction rate than not rotatable reactor；Conversely, dioxy
Change titanium（TiO2）The intermediary material desorption of Surface Creation is drawn up, low when causing reaction rate than not rotatable reactor.
So, it is possible to use the mass loss Δ m that DTG measures sample in the unit interval judges reaction rate to judge in the middle of reaction
The surface that media material is preferentially formed.
The above embodiment of the present invention is only example to illustrate the invention, and is not the implementation to the present invention
The restriction of mode.For those of ordinary skill in the field, other can also be made not on the basis of the above description
With the change and variation of form.Here all embodiments can not be exhaustive.It is every to belong to technical scheme
Row of the obvious changes or variations amplified out still in protection scope of the present invention.
Claims (9)
1. a kind of surface reaction detection device, it is characterised in that including vacuum atmosphere furnace system, mass measurement system and electromagnetic rotating
System；
Described vacuum atmosphere furnace system includes boiler tube, furnace shell and heating mantle；Described furnace shell is in integrally the casing of inner hollow,
Described heating mantle is enclosed on outside furnace shell, for giving the heating of vacuum atmosphere furnace system；Described furnace shell top is provided with blast pipe；
Mounting hole is also provided with the top of described furnace shell, for being socketed described boiler tube；Described boiler tube is that the entirety being vertically arranged is presented
End face closed lower face is open tubular, and the boiler tube is fastened in furnace shell, between the opening and the inner bottom surface of furnace shell of tubular
Space is left, described boiler tube and the inner space of furnace shell constitute the confined space that can be evacuated；Described boiler tube
The center of top surface is provided with the connecting hole for quality of connection measuring system；Described boiler tube top is connected with air inlet pipe I and air inlet
Pipe II, the air inlet pipe I and air inlet pipe II extend to inside the boiler tube and the mouth of pipe straight down；
Described mass measurement system includes mass sensor, suspension wire, inverted U-shaped suspension ring, bearing connector, connecting rod and loading
Rotor；The mass sensor can detect the change of the material mass being hung below and quality；Described suspension wire
It is vertically arranged, its upper end is fixedly connected with mass sensor, lower end and the peak of inverted U-shaped suspension ring are detachably connected to one
Rise, described bearing connector is fixed in two ring arm of the inverted U-shaped suspension ring；Described connecting rod is vertically arranged, and its upper end can
Rotationally it is connected with bearing connector, can keeps inverted U-shaped suspension ring static when connecting rod horizontally rotates, described connecting rod passes through position
Connecting hole in boiler tube top surface center is extended in the boiler tube, and the lower end of described connecting rod is fixed on the center of the loading rotor
Point；The loading rotor is the shape of horizontally disposed entirety axisymmetricly, can be carried under the driving of electromagnetic rotating system
The central point of thing rotor horizontally rotates for pivot；
Described electromagnetic rotating system is arranged on the lower section of described furnace shell bottom, including motor and driving rotor；The drive of motor
Moving axis is vertically arranged, and can be horizontally rotated under the driving of motor, and the top of the drive shaft is fixed in the driving rotor
Heart point, the driving rotor is the shape of horizontally disposed entirety axisymmetricly, can drive rotor under the driving of motor
Central point horizontally rotates for pivot, and drives loading rotor to rotate in the presence of magnetic force induction.
2. reaction detection device in surface according to claim 1, it is characterised in that described boiler tube is in the dumbbell being vertically arranged
Shape, inside is a dumb-bell shape cavity, and the bottom of boiler tube is opening, dumb-bell shape cavity to be connected with furnace shell inner space.
3. reaction detection device in surface according to claim 1, it is characterised in that described bearing connector is by being horizontally disposed with
Bearing I and bearing II constitute, described bearing I and the line of centres of bearing II and the central axis of connecting rod are in a plumb line
On, connecting rod can be made not shift and rock when horizontally rotating.
4. reaction detection device in surface according to claim 2, it is characterised in that described connecting rod is upper and lower two sections, two sections
Between be removably joined together；Described boiler tube top surface is provided with a dress sample hole, and dress sample hole overlying has described for closing
The closure of boiler tube, the closure is detachably connected to the top surface of the boiler tube.
5. reaction detection device in surface according to claim 1, it is characterised in that described loading rotor and sample gap
Correspondence position is provided with several equidistant diameter 1mm vertical through holes.
6. according to any described surface reaction detection devices of claim 1-5, it is characterised in that set in described blast pipe
There is check valve, the check valve is only capable of to the side opening opposite with furnace shell.
7. according to any described surface reaction detection device of claim 6, it is characterised in that the amount of described mass sensor
Journey is 0~300g, and accuracy is 0.5mg.
8. according to any described surface reaction detection device of claim 6, it is characterised in that described heating mantle by body and
Resistant heating body composition inside body.
9. a kind of method for detecting the reaction of titanium dioxide carburizing chlorination, it is characterised in that usage right requires any described in 1-8
Surface reaction detection device, its step includes：
1）Sample preparation：Sample is made, the sample includes two pieces of annular coupons I, coupon II and some platinum pieces；Described examination
The internal diameter of sample block I is identical with the external diameter of described connecting rod, and the internal diameter of described coupon II is more than the external diameter of coupon I, sample
The diameter of block II is less than the length of described loading rotor；Described coupon I is placed in the ring of coupon II, platinum piece card
Between coupon I and coupon II；Wherein coupon I is made up of carbon, and coupon II is made up of titanium dioxide；
2）Be powered preheating：Open heating mantle to heat vacuum atmosphere furnace system, by the way of gradually heating up, be warming up to
900 DEG C are preheated, and preheating time is not less than 30 minutes；
3）Fill sample：Coupon I on sample is enclosed on connecting rod and fallen on loading rotor, is then slowly put into boiler tube, will
In-furnace temperature rises to 1000 DEG C of reaction temperature, and keeps constant；
4）Ventilation：First the air in the confined space of vacuum atmosphere furnace system is evacuated down to by described blast pipe-
0.097MPa；Air inlet pipe II is connected into argon bottle again, argon gas is injected into boiler tube with 2L/min flow；
The initial mass m of sample is measured and recorded by mass sensor1, then air inlet pipe I connected into chlorine cylinder, with 2L/min's
Flow injects chlorine into boiler tube, carries out chlorination reaction；Record the mass change Δ m in the sample unit interval1, under the conditions of this
Carburizing chlorination reaction rate is designated as Δ m1/Δt；
5）Speed governing is detected：By the electric motor starting of described electromagnetic rotating system, and regulation motor rotating speed is so that turn of loading rotor
Speed is constant, the mass change Δ m in the record sample unit interval2, the carburizing chlorination reaction rate under centrifugal forces affect is remembered
For Δ m2/Δt；
6）Shutdown：Motor, heating mantle and chlorine cylinder are first closed, by air inlet pipe II into the confined space of vacuum atmosphere furnace system
Continue logical argon gas, until the quality that mass sensor is detected no longer changes；
7）Interpretation of result：If the carburizing chlorination reaction rate Δ m under having centrifugal action2/ Δ t is more than under inactive state plus carbon
Chlorination reaction speed Δ m1During/Δ t, illustrate that intermediate medium is generated in carbon surface；If Δ m2/ Δ t is less than Δ m1During/Δ t, explanation
Intermediate medium is generated in titanium dioxide surface.
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