CN105067470A - Surface reaction detector and detection method thereof - Google Patents
Surface reaction detector and detection method thereof Download PDFInfo
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- CN105067470A CN105067470A CN201510426299.1A CN201510426299A CN105067470A CN 105067470 A CN105067470 A CN 105067470A CN 201510426299 A CN201510426299 A CN 201510426299A CN 105067470 A CN105067470 A CN 105067470A
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Abstract
The invention provides a surface reaction detector and a detection method thereof. The surface reaction detector comprises a vacuum atmosphere furnace system, a mass measuring system and an electromagnetic rotation system, wherein a carrying rotor of the mass measuring system is driven to rotate horizontally under the drive action of the electromagnetic rotation system, the defect that to-be-detected samples are required to be static in the existing thermogravimetric technique is overcome, and the existing thermogravimetric technique is improved into a dynamic thermogravimetric technique in which samples with carbon inside and titanium dioxide outside have controllable self-rotation movement in the chlorine atmosphere so as to realize dynamic measurement. By means of the detection method, the mass loss delta m of the samples per unit time is measured with the thermogravimetric method under the action of centrifugal force, so that surfaces formed by reaction intermediate medium substances preferentially are judged through calculation of reaction rates, and an important basis is provided for further research on forming ways of intermediate media of titanium oxide carbochlorination reactions.
Description
Technical field
The invention belongs to surface reaction process detection technical field, be specifically related to a kind of method of surface reaction detecting device and detection thereof.
Background technology
According to oxygen gesture figure and the chlorine gesture figure of metal oxide, titanium oxide, particularly titania directly to be changed into muriatic by the chlorination of chlorine institute.But deposit in case at reductive agents such as having carbon, make the chlorination of titania become possibility, and the reactivity worth of itself and chlorine has and improves significantly.Carburizing chlorination reaction is a gas phase and two solid phases---TiO
2, the heterogeneous reaction of complexity that participates in of C.Domestic and international experts and scholars have carried out large quantity research to it, successively propose the viewpoint of this macroscopic appearance of many explanations, and a class viewpoint thinks TiO
2first TiCl is chlorinated into again after being reduced to titanium suboxide by C
4.But under actual chlorination furnace temperature of reaction condition, the probability that the direct-reduction effect of C produces is very micro-, TiO
2the speed being reduced to titanium suboxide by carbon is very low, can not explain that carburizing chlorination reaction rate significantly improves this fact.Another kind of viewpoint thinks the existence having intermediate product and intermediate medium, although TiO
2with Cl
2the standard free enthalpy of reaction be on the occasion of, but in reaction system, still have the TiCl of minute quantity
4produce, the TiCl of this minute quantity just
4be adsorbed on TiO
2the intermediate product of Surface Creation more further with C and Cl
2react and define final product TiCl
4; In addition, reductive agent C and the O added also is thought
2reaction can reduce the partial pressure of oxygen that chlorination is formed, and solid carbon changes CO into, and Cl
2react with CO and generate COCl or COCl
2after intermediate product, then with TiO
2there is chlorination reaction and form product TiCl
4.
In a word, above-mentioned viewpoint is all based on thermodynamic analysis to the explanation of macroscopic appearance and supposition, and its key point determines Cl
2, TiO
2and the intermediate medium of this reaction of promotion of reaction sequence between C three and generation.Therefore exploitation can detect instrument and the experimental technique of surface reaction speed, and for this type of surface reaction of research, tool is of great significance.
Summary of the invention
For prior art above shortcomings, the invention provides a kind of method of surface reaction detecting device and detection thereof, can make to cause intermediate medium to become controlled reaction process on carbon granule surface and the titanium oxide adsorption Low Response opposite sex by the present invention, to reach the carburizing chlorination reaction formation of intermediate medium of research titanium oxide and the object of pipeline.
To achieve these goals, the technical solution used in the present invention is as follows:
A kind of surface reaction detecting device, comprises vacuum atmosphere furnace system, mass measurement system and electromagnetic rotating system; Described vacuum atmosphere furnace system comprises boiler tube, furnace shell and heating jacket; The described casing of furnace shell entirety in inner hollow, described heating jacket is enclosed within furnace shell outside, for giving vacuum atmosphere oven system heating; Described furnace shell top is provided with gas outlet; Described furnace shell top also has mounting hole, for being socketed described boiler tube; Described boiler tube is the entirety that vertically arranges be closed lower face, upper surface is uncovered tubular, this boiler tube is fastened in furnace shell, leave space between the uncovered and inner bottom surface of furnace shell of tubular, described boiler tube and the inner space of furnace shell constitute can evacuated confined space; The central authorities of the end face of described boiler tube have the connecting hole for quality of connection measuring system; Described boiler tube top is connected with draft tube I and draft tube II, and described draft tube I and draft tube II extend to the inner and mouth of pipe of described boiler tube straight down; Described mass measurement system comprises mass sensor, suspension wire, inverted U-shaped suspension ring, bearing connector, connecting rod and load sample rotor; Described mass sensor can detect suspension material mass thereunder and the change of quality; Described suspension wire is vertically arranged, and its upper end is fixedly connected with mass sensor, and the peak of lower end and inverted U-shaped suspension ring removably links together, and described bearing connector is fixed in two ring arm of described inverted U-shaped suspension ring; Described connecting rod is vertically arranged, its upper end is connected with bearing connector rotationally, inverted U-shaped suspension ring can be kept static when connecting rod horizontally rotates, described connecting rod extends to this boiler tube by the connecting hole being positioned at boiler tube end face central authorities, and the lower end of described connecting rod is fixed on the central point of described loading rotor; Described loading rotor is horizontally disposed entirety shape axisymmetricly, can under the driving of electromagnetic rotating system with the central point of loading rotor for rotation center horizontally rotates; The described below of electromagnetic rotating Operation system setting bottom described furnace shell, comprises motor and drives rotor; The driving shaft of motor is vertically arranged, can horizontally rotate under the driving of motor, the top of this driving shaft is fixed on the central point of described driving rotor, this driving rotor is horizontally disposed entirety shape axisymmetricly, to drive the central point of rotor to horizontally rotate for rotation center under the driving of motor, and loading rotor turns can be driven under the effect of magnetic force induction.
Further, described boiler tube is in the dumb-bell shape vertically arranged, and inside is a dumb-bell shape cavity, and the bottom of boiler tube is uncovered, in order to be communicated with furnace shell inner space by dumb-bell shape cavity.
Further, described bearing connector is made up of horizontally disposed bearing I and bearing II, and described bearing I and the line of centres of bearing II and the central axis of connecting rod, on a pedal line, can make connecting rod skew not occur when horizontally rotating and rock.
Further, described connecting rod is upper and lower two sections, removably links together between two sections; Described boiler tube end face has a dress sample hole, and dress sample hole is covered with the gland bonnet for closing described boiler tube, sealing lid is removably connected to the end face of described boiler tube.
Further, described load sample rotor and the correspondence position in sample gap have the vertical through holes of several equidistant diameter 1mm.
Further, be provided with retaining valve in described gas outlet, described retaining valve only can be opened to the side opposing with furnace shell.
Further, the range of described mass sensor is 0 ~ 300g, and degree of accuracy is 0.5mg.
Further, described heating jacket is made up of the Resistant heating body of body and body inside.
With above-mentioned surface reaction detecting device with the use of a sample, comprise two pieces of annular coupon I, coupon II and some platinum sheets; 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 greater than the external diameter of coupon I, and the diameter of coupon II is less than the length of described loading rotor; Described coupon I is placed in the ring of coupon II, and platinum sheet is stuck between coupon I and coupon II.
Detect a method for titania carburizing chlorination reaction, this method uses above-mentioned surface reaction detecting device, and its step comprises:
1) sample preparation: the sample making claim 9, wherein coupon I is made up of carbon, and coupon II is made up of titania;
2) be energized preheating: open heating jacket and heat vacuum atmosphere furnace system, adopt the mode heated up gradually, be warming up to 900 DEG C and carry out preheating, be not less than 30 minutes preheating time;
3) sample is filled: to be enclosed within by the coupon I on sample on connecting rod and to drop on loading rotor, then slowly putting into boiler tube, in-furnace temperature is risen to temperature of reaction 1000 DEG C, and remain unchanged;
4) ventilate: first the air in the confined space of vacuum atmosphere furnace system is evacuated down to-0.097MPa by described gas outlet; Again draft tube II is connected argon bottle, in boiler tube, inject argon gas with the flow of 2L/min;
Measured by mass sensor and record the initial mass m of sample
1, then draft tube I is connected chlorine cylinder, in boiler tube, inject chlorine with the flow of 2L/min, carry out chlorination reaction; Mass change Δ m in the record sample unit interval
1, carburizing chlorination reaction rate under this condition is designated as Δ m
1/ Δ t;
5) speed governing detects: by the electric motor starting of described electromagnetic rotating system, and regulate motor speed to make the rotating speed of loading rotor constant, the mass change Δ m in the record sample unit interval
2, the carburizing chlorination reaction rate under centrifugal forces affect is designated as Δ m
2/ Δ t;
6) shut down: first disable motor, heating jacket and chlorine cylinder, in the confined space of vacuum atmosphere furnace system, continue logical argon gas, until the quality that mass sensor detects no longer changes by draft tube II;
7) interpretation of result: if the carburizing chlorination reaction rate Δ m under having centrifugal action
2/ Δ t is greater than the carburizing chlorination reaction rate Δ m under stationary state
1during/Δ t, illustrate that intermediate medium generates at carbon surface; If Δ m
2/ Δ t is less than Δ m
1during/Δ t, illustrate that intermediate medium generates at titanium dioxide surface.
Compared with prior art, the present invention has following beneficial effect:
1, by under the effect of electromagnetic rotating, overcome in existing thermogravimetric technology the defect requiring that tested sample must be static, existing thermogravimetric technique improvement is become a kind of dynamic thermogravimetric technology that the sample of inner ring carbon outer shroud titania can be made in chlorine atmosphere to carry out controlled spinning campaign.
2, under the influence of centrifugal force, this thermogravimetry (TG) is utilized to record the mass loss Δ m of sample in the unit interval, and then calculating reaction rate judges the surface that reaction intermediate medium material is preferentially formed, for the forming feature of the intermediate medium studying the reaction of titanium oxide carburizing chlorination further provides important evidence.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention;
Fig. 2 is sample mounting structure cut-open view of the present invention.
In accompanying drawing: 1-mass sensor; 2-suspension wire; 3-inverted U-shaped suspension ring; 4-bearing I; 5-draft tube I; 6-furnace shell; 7-heating jacket; 8-drive rotor; 9-motor; 10-load sample rotor; 11-sample; 12-connecting rod; 13-gas outlet; 14-boiler tube; 15-draft tube II; 16-bearing II.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail.
As shown in Figure 1, a kind of surface reaction detecting device, is characterized in that, comprises vacuum atmosphere furnace system, mass measurement system and electromagnetic rotating system;
Described vacuum atmosphere furnace system comprises boiler tube 14, furnace shell 6 and heating jacket 7; The described casing of furnace shell 6 entirety in inner hollow, it is outside that described heating jacket 7 is enclosed within furnace shell 6, for giving vacuum atmosphere oven system heating; Described furnace shell 6 top is provided with gas outlet 13; Described furnace shell 6 top also has mounting hole, for being socketed described boiler tube 14; Described boiler tube 14 is the entirety that vertically arranges be closed lower face, upper surface is uncovered tubular, this boiler tube 14 is fastened in furnace shell 6, leave space between the inner bottom surface of the uncovered and furnace shell 6 of tubular, described boiler tube 14 and the inner space of furnace shell 6 constitute can evacuated confined space; The central authorities of the end face of described boiler tube have the connecting hole for quality of connection measuring system; Described boiler tube 14 top is connected with draft tube I 5 and draft tube II 15, and described draft tube I 5 and draft tube II 15 extend to the inner and mouth of pipe of described boiler tube 14 straight down;
Described mass measurement system comprises mass sensor 1, suspension wire 2, inverted U-shaped suspension ring 3, bearing connector, connecting rod 12 and load sample rotor 10; Described mass sensor 1 can detect suspension material mass thereunder and the change of quality; Described suspension wire 2 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 removably links together, and described bearing connector is fixed in two ring arm of described inverted U-shaped suspension ring 3; Described connecting rod 12 is vertically arranged, its upper end is connected with bearing connector rotationally, inverted U-shaped suspension ring 3 can be kept static when connecting rod horizontally rotates, described connecting rod 12 extends to this boiler tube 14 by the connecting hole being positioned at boiler tube 14 end face central authorities, and the lower end of described connecting rod 12 is fixed on the central point of described loading rotor 10; Described loading rotor 10 is horizontally disposed entirety shape axisymmetricly, can under the driving of electromagnetic rotating system with the central point of loading rotor 10 for rotation center horizontally rotates;
The below of described electromagnetic rotating Operation system setting bottom described furnace shell 6, comprises motor 9 and drives rotor 8; The driving shaft of motor 9 is vertically arranged, can horizontally rotate under the driving of motor 9, the top of this driving shaft is fixed on the central point of described driving rotor 8, this driving rotor 8 is horizontally disposed entirety shape axisymmetricly, can to drive the central point of rotor 8 to horizontally rotate for rotation center under the driving of motor 9, and under the effect of magnetic force induction, loading rotor 10 be driven to rotate.
As one preferred embodiment, described boiler tube 14 is in the dumb-bell shape vertically arranged, and inside is a dumb-bell shape cavity, and the bottom of boiler tube 14 is uncovered, in order to be communicated with furnace shell 6 inner space by dumb-bell shape cavity.Boiler tube is designed shape for this reason, the scope that reacting gas and sample can be made to meet in boiler tube is less, to make reaction more abundant.
As one preferred embodiment, described bearing connector is made up of horizontally disposed bearing I 4 and bearing II 16, the line of centres of bearing I 4 and bearing II 16 and the central axis of connecting rod, on a pedal line, can make connecting rod skew not occur when horizontally rotating and rock.
As one preferred embodiment, for the ease of being sleeved on connecting rod 12 by sample 11, described connecting rod 12 is upper and lower two sections, removably links together between two sections; In order to load sample 11 when not taking off boiler tube 14, can open a dress sample hole at described boiler tube 14 end face, dress sample hole is covered with the gland bonnet for closing described boiler tube, sealing lid is removably connected to the end face of described boiler tube.
As one preferred embodiment, conveniently react with sample 11 to make chlorine and discharge in time and react afterproduct, have the vertical through holes of several equidistant diameter 1mm at described load sample rotor 10 and the correspondence position in sample 11 gap.
As one preferred embodiment, be provided with retaining valve in described gas outlet 13, described retaining valve only can be opened to the side opposing with furnace shell, so that the gas that the discharge air of orientation and reaction produce, and anti-backflow.
As one preferred embodiment, in order to the requirement making accuracy of detection meet experiment, described mass sensor 1 should select the mass sensitivity equipment that range is 0 ~ 300g, degree of accuracy is 0.5mg.
As one preferred embodiment, described heating jacket 7 is made up of the Resistant heating body of body and body inside.
A kind of and above-mentioned surface reaction detecting device with the use of sample 11, it is characterized in that, comprise two pieces of annular coupon I, coupon II and some platinum sheets; 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 greater than the external diameter of coupon I, and the diameter of coupon II is less than the length of described loading rotor; Described coupon I is placed in the ring of coupon II, and platinum sheet is stuck between coupon I and coupon II, remains unchanged to make distance therebetween.
Detect a method for titania carburizing chlorination reaction, it is characterized in that, employ above-mentioned surface reaction detecting device and sample 11, its step comprises:
1) sample preparation: carbon is made coupon I, makes coupon II by titania, then platinum sheet is stuck between coupon I and coupon II, remains unchanged to make distance therebetween;
2) be energized preheating: open heating jacket 7 pairs of vacuum atmosphere furnace systems and heat, adopt the mode heated up gradually, be warming up to 900 DEG C and carry out preheating, be not less than 30 minutes preheating time;
3) sample is filled: inserted by the sample 11 made in connecting rod and fix as shown in Figure 2, and slowly put into boiler tube 14, temperature is risen to temperature of reaction 1000 DEG C, and remain unchanged;
4) ventilate: first the air in the confined space of vacuum atmosphere furnace system is evacuated down to-0.097MPa by described gas outlet 13; Again draft tube II 15 is connected argon bottle, in boiler tube 14, inject argon gas with the flow of 2L/min;
Measured by mass sensor 1 and record the initial mass m1 of sample 11, then draft tube I 5 is connected chlorine cylinder, in boiler tube 14, injecting chlorine with the flow of 2L/min, carry out chlorination reaction; Mass change Δ m in record sample 11 unit interval
1, carburizing chlorination reaction rate under this condition is designated as Δ m
1/ Δ t;
5) speed governing detects: started by the motor 9 of described electromagnetic rotating system, and regulate motor 9 rotating speed to make the rotating speed of loading rotor 10 constant, the mass change Δ m in record sample 11 unit interval
2, the carburizing chlorination reaction rate under centrifugal forces affect is designated as Δ m
2/ Δ t;
6) shut down: first disable motor, heating jacket and chlorine cylinder, in the confined space of vacuum atmosphere furnace system, continue logical argon gas, until the quality that mass sensor detects no longer changes by draft tube II;
7) interpretation of result: if the carburizing chlorination reaction rate Δ m under having centrifugal action
2/ Δ t is greater than the carburizing chlorination reaction rate Δ m under stationary state
1during/Δ t, illustrate that intermediate medium generates at carbon surface; If Δ m
2/ Δ t is less than Δ m
1during/Δ t, illustrate that intermediate medium generates at titanium dioxide surface.
In order to increase the accuracy of experimental result, the mass change Δ m in the unit interval under step 5) record different rotating speeds can be repeated
3Δ m
nwith the carburizing chlorination reaction rate Δ m under centrifugal forces affect
3/ Δ t ... Δ m
n/ Δ t; According to the mass change Δ m in the unit interval
1Δ m
nwith the carburizing chlorination reaction rate Δ m under centrifugal forces affect
1/ Δ t ... Δ m
n/ Δ t analyzes testing result.If the carburizing chlorination reaction rate Δ m under having centrifugal action
2/ Δ t ... Δ m
n/ Δ t is greater than the carburizing chlorination reaction rate Δ m under stationary state
1during/Δ t, illustrate that intermediate medium generates at carbon surface; If Δ m
2/ Δ t ... Δ m
n/ Δ t is less than Δ m
1during/Δ t, illustrate that intermediate medium generates at titanium dioxide surface.
The material of sample coupon I and coupon II can be exchanged, and the test findings inference method after exchange is identical.
Cleaning Principle of the present invention: because the mass sensor measuring accuracy of thermogravimetry (TG) is higher, motor 9 cannot directly be connected with rotor, so design motor 9 is connected with driving rotor 8, drive rotor 8 to drive loading rotor 10 to rotate by electromagnetic force, and realize motor 9 and indirect connection of rotor and thermogravimetry (TG) is carried out smoothly.Experimentally can need the rotational speed adjusting motor, under the effect of rotary centrifugal force, the intermediary material desorption rate that carbon (C) generates on the surface improves, and more easily arrives titania (TiO
2) surface, high when reaction rate can be made to react than non rotating; Otherwise, titania (TiO
2) the intermediary material desorption of Surface Creation drawn up, and causes reaction rate than low during non rotating reactor.Like this, the mass loss Δ m that thermogravimetry (TG) can be utilized to record sample in the unit interval judges reaction rate to judge to react the middle intermediary surface first formed of fine quality.
According to carburizing chlorination reaction equation, reaction generates gas TiCl
4, CO
2and CO, the quality of carbon and titania sample can reduce gradually along with the carrying out of reaction, and its reaction rate can calculate according to the mass loss Δ m of sample in the unit interval, add carbon and promote that the essence of titania chlorination reaction is, therebetween generate intermediary, experimentally can need the rotational speed adjusting motor, under the effect of rotary centrifugal force, the intermediary material desorption rate that carbon (C) generates on the surface improves, and more easily arrives titania (TiO
2) surface, reaction rate can be made than high during non rotating reactor; Otherwise, titania (TiO
2) the intermediary material desorption of Surface Creation drawn up, and causes reaction rate than low during non rotating reactor.Like this, the mass loss Δ m that thermogravimetry (TG) can be utilized to record sample in the unit interval judges reaction rate to judge to react the middle intermediary surface first formed of fine quality.
The above embodiment of the present invention is only for example of the present invention is described, and is not the restriction to embodiments of the present invention.For those of ordinary skill in the field, other multi-form change and variations can also be made on the basis of the above description.Here cannot give exhaustive to all embodiments.Every belong to technical scheme of the present invention the apparent change of amplifying out or variation be still in the row of protection scope of the present invention.
Claims (10)
1. a surface reaction detecting device, is characterized in that, comprises vacuum atmosphere furnace system, mass measurement system and electromagnetic rotating system;
Described vacuum atmosphere furnace system comprises boiler tube, furnace shell and heating jacket; The described casing of furnace shell entirety in inner hollow, described heating jacket is enclosed within furnace shell outside, for giving vacuum atmosphere oven system heating; Described furnace shell top is provided with gas outlet; Described furnace shell top also has mounting hole, for being socketed described boiler tube; Described boiler tube is the entirety that vertically arranges be closed lower face, upper surface is uncovered tubular, this boiler tube is fastened in furnace shell, leave space between the uncovered and inner bottom surface of furnace shell of tubular, described boiler tube and the inner space of furnace shell constitute can evacuated confined space; The central authorities of the end face of described boiler tube have the connecting hole for quality of connection measuring system; Described boiler tube top is connected with draft tube I and draft tube II, and described draft tube I and draft tube II extend to the inner and mouth of pipe of described boiler tube straight down;
Described mass measurement system comprises mass sensor, suspension wire, inverted U-shaped suspension ring, bearing connector, connecting rod and load sample rotor; Described mass sensor can detect suspension material mass thereunder and the change of quality; Described suspension wire is vertically arranged, and its upper end is fixedly connected with mass sensor, and the peak of lower end and inverted U-shaped suspension ring removably links together, and described bearing connector is fixed in two ring arm of described inverted U-shaped suspension ring; Described connecting rod is vertically arranged, its upper end is connected with bearing connector rotationally, inverted U-shaped suspension ring can be kept static when connecting rod horizontally rotates, described connecting rod extends to this boiler tube by the connecting hole being positioned at boiler tube end face central authorities, and the lower end of described connecting rod is fixed on the central point of described loading rotor; Described loading rotor is horizontally disposed entirety shape axisymmetricly, can under the driving of electromagnetic rotating system with the central point of loading rotor for rotation center horizontally rotates;
The described below of electromagnetic rotating Operation system setting bottom described furnace shell, comprises motor and drives rotor; The driving shaft of motor is vertically arranged, can horizontally rotate under the driving of motor, the top of this driving shaft is fixed on the central point of described driving rotor, this driving rotor is horizontally disposed entirety shape axisymmetricly, to drive the central point of rotor to horizontally rotate for rotation center under the driving of motor, and loading rotor turns can be driven under the effect of magnetic force induction.
2. surface reaction detecting device according to claim 1, is characterized in that, described boiler tube is in the dumb-bell shape vertically arranged, and inside is a dumb-bell shape cavity, and the bottom of boiler tube is uncovered, in order to be communicated with furnace shell inner space by dumb-bell shape cavity.
3. surface reaction detecting device according to claim 1, it is characterized in that, described bearing connector is made up of horizontally disposed bearing I and bearing II, described bearing I and the line of centres of bearing II and the central axis of connecting rod, on a pedal line, can make connecting rod skew not occur when horizontally rotating and rock.
4. surface reaction detecting device according to claim 2, is characterized in that, described connecting rod is upper and lower two sections, removably links together between two sections; Described boiler tube end face has a dress sample hole, and dress sample hole is covered with the gland bonnet for closing described boiler tube, sealing lid is removably connected to the end face of described boiler tube.
5. surface reaction detecting device according to claim 1, is characterized in that, described load sample rotor and the correspondence position in sample gap have the vertical through holes of several equidistant diameter 1mm.
6. arbitrary surface reaction detecting device according to claim 1, is characterized in that, be provided with retaining valve in described gas outlet, and described retaining valve only can be opened to the side opposing with furnace shell.
7. the arbitrary surface reaction detecting device according to claim 1-6, is characterized in that, the range of described mass sensor is 0 ~ 300g, and degree of accuracy is 0.5mg.
8. the arbitrary surface reaction detecting device according to claim 1-6, is characterized in that, described heating jacket is made up of the Resistant heating body of body and body inside.
9. the sample used in claim 1, is characterized in that, comprises two pieces of annular coupon I, coupon II and some platinum sheets; 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 greater than the external diameter of coupon I, and the diameter of coupon II is less than the length of described loading rotor;
Described coupon I is placed in the ring of coupon II, and platinum sheet is stuck between coupon I and coupon II.
10. detect a method for titania carburizing chlorination reaction, it is characterized in that, use arbitrary described surface reaction detecting device in claim 1-8, its step comprises:
1) sample preparation: the sample making claim 9, wherein coupon I is made up of carbon, and coupon II is made up of titania;
2) be energized preheating: open heating jacket and heat vacuum atmosphere furnace system, adopt the mode heated up gradually, be warming up to 900 DEG C and carry out preheating, be not less than 30 minutes preheating time;
3) sample is filled: to be enclosed within by the coupon I on sample on connecting rod and to drop on loading rotor, then slowly putting into boiler tube, in-furnace temperature is risen to temperature of reaction 1000 DEG C, and remain unchanged;
4) ventilate: first the air in the confined space of vacuum atmosphere furnace system is evacuated down to-0.097MPa by described gas outlet; Again draft tube II is connected argon bottle, in boiler tube, inject argon gas with the flow of 2L/min;
Measured by mass sensor and record the initial mass m of sample
1, then draft tube I is connected chlorine cylinder, in boiler tube, inject chlorine with the flow of 2L/min, carry out chlorination reaction; Mass change Δ m in the record sample unit interval
1, carburizing chlorination reaction rate under this condition is designated as Δ m
1/ Δ t;
5) speed governing detects: by the electric motor starting of described electromagnetic rotating system, and regulate motor speed to make the rotating speed of loading rotor constant, the mass change Δ m in the record sample unit interval
2, the carburizing chlorination reaction rate under centrifugal forces affect is designated as Δ m
2/ Δ t;
6) shut down: first disable motor, heating jacket and chlorine cylinder, in the confined space of vacuum atmosphere furnace system, continue logical argon gas, until the quality that mass sensor detects no longer changes by draft tube II;
7) interpretation of result: if the carburizing chlorination reaction rate Δ m under having centrifugal action
2/ Δ t is greater than the carburizing chlorination reaction rate Δ m under stationary state
1during/Δ t, illustrate that intermediate medium generates at carbon surface; If Δ m
2/ Δ t is less than Δ m
1during/Δ t, illustrate that intermediate medium generates at titanium dioxide surface.
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| CN112588211A (en) * | 2021-01-18 | 2021-04-02 | 重庆大学 | Titanium dioxide carbonization boiling chlorination simulation reactor and simulation method |
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