CN106117594A - Waste old microwave automatic cracking reaction device - Google Patents
Waste old microwave automatic cracking reaction device Download PDFInfo
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- CN106117594A CN106117594A CN201610590076.3A CN201610590076A CN106117594A CN 106117594 A CN106117594 A CN 106117594A CN 201610590076 A CN201610590076 A CN 201610590076A CN 106117594 A CN106117594 A CN 106117594A
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- silicon chip
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J11/00—Recovery or working-up of waste materials
- C08J11/04—Recovery or working-up of waste materials of polymers
- C08J11/10—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2319/00—Characterised by the use of rubbers not provided for in groups C08J2307/00 - C08J2317/00
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
Abstract
The invention discloses waste old microwave automatic cracking reaction device, including device body and frequency conversion motor；Described frequency conversion motor is connected with the rotary shaft of device body；Described rotary shaft runs through described device body and the axial direction along described device body extends；It is connected in the described rotary shaft of side with described frequency conversion motor and is provided with rotation shaft seal；Described rotary shaft is provided around matched spiral propeller；Described rotary shaft side is provided with microwave magnetron；The shell side of described device body is disposed with the first manhole, cracking gas floss hole, the second manhole and rubber raw materials entrance, and opposite side is provided with the connecting tube for being connected with other cracking reaction devices；Described device body is fixedly provided with detector.
Description
Technical field
The present invention relates to waste rubber cracking device, particularly relate to waste old microwave automatic cracking reaction device.
Background technology
During waste old recycles, will can produce substantial amounts of toxic gas, phase during waste rubber cracking
There is volume and cause greatly the problem that maintenance cost is high in the cracker used in the technology of pass.
Summary of the invention
It is desirable to provide waste old microwave automatic cracking reaction device, to solve above-mentioned technical problem.
Embodiments of the invention provide waste old microwave automatic cracking reaction device, including device body and frequency conversion
Motor；Described frequency conversion motor is connected with the rotary shaft of device body；Described rotary shaft runs through described device body and along described dress
The axial direction putting body extends；It is connected in the described rotary shaft of side with described frequency conversion motor and is provided with rotation shaft seal；
Described rotary shaft is provided around matched spiral propeller；Described rotary shaft side is provided with microwave magnetron；Described
The shell side of device body is disposed with the first manhole, cracking gas floss hole, the second manhole and rubber raw materials
Entrance, opposite side is provided with the connecting tube for being connected with other cracking reaction devices；Described device body is fixedly provided with gas
Detector.
The cracking reaction apparatus structure that the above embodiment of the present invention provides arranges rationally, further reduces cracking dress
The volume put, thus solve above-mentioned technical problem.
Accompanying drawing explanation
Accompanying drawing herein is merged in description and constitutes the part of this specification, it is shown that meet the enforcement of the present invention
Example, and for explaining the principle of the present invention together with description.
Fig. 1 is the structural representation of the present invention.
Fig. 2 is the structural representation of the detector used according to the present invention shown in an exemplary embodiment.
The structural representation of the sensitive blocks that Fig. 3 uses according to the present invention shown in an exemplary embodiment.
Fig. 4 is the preparation technology FB(flow block) of the sensitive blocks used according to the present invention shown in an exemplary embodiment.
Wherein: 1-silicon chip, 2-silicon nitride layer, 3-Cr film layer, 4-PANI film, 5-Ni film, 6-HKUST-1 film, 7-BSP film,
8-device body, 9-the first manhole, 10-sensitive blocks, 11-cracking gas floss hole, 12-the second manhole, 13-rubber
Feed(raw material)inlet, 14-microwave magnetron, 18-rotation shaft seal, 19-frequency conversion motor, 20-data read module, 21-gas is examined
Survey device, 22-spiral propeller, 23-connecting tube.
Detailed description of the invention
Here will illustrate exemplary embodiment in detail, its example represents in the accompanying drawings.Explained below relates to
During accompanying drawing, unless otherwise indicated, the same numbers in different accompanying drawings represents same or analogous key element.Following exemplary embodiment
Described in embodiment do not represent all embodiments consistent with the present invention.On the contrary, they are only with the most appended
The example of the apparatus and method that some aspects that described in detail in claims, the present invention are consistent.
In the description of the present application, it should be noted that unless otherwise prescribed and limit, term " is installed ", " being connected ",
" connect " and should be interpreted broadly, for example, it may be mechanically connected or electrical connection, it is also possible to be the connection of two element internals, can
Being to be joined directly together, it is also possible to be indirectly connected to by intermediary, for the ordinary skill in the art, can basis
Concrete condition understands the concrete meaning of above-mentioned term.
Along with economic fast development and industrial expansion, not only can produce various in industry manufactures production process
The waste gas of various kinds, the most also can produce various gas at the various apparatuses made, and the generation of these gases not only can
Affect the use of instrument itself, and the potential threat of environmental pollution can be become.
Therefore, it is necessary to look for a kind of equipment that can monitor the gas that various apparatus in use produces, again may be used
Gas sensor with timely feedback monitoring to gas data.
The method of conventional detected gas is to gather gas at the scene, is stored in the sample devices of cleaning, is then sent to
Laboratory, uses the composition in the detected gas such as various instrument, such as GC, GC/MS or LC/MS and the problem such as quantitatively, but,
Above-mentioned detection method not only needs substantial amounts of sample collector to carry out spot sampling, consumes substantial amounts of manpower and materials, and at sample
In product transportation, it is frequently present of contaminated problem, delivers to the gaseous sample of laboratory and can not exist by reactor tool at all
Problem, maybe can not monitor its hazardness to environmental functional.
In existing report, there is employing inorganic material film and made gas detection sensor and carry out detected gas, but
That above-mentioned gas sensor there is problems in that the membrane material of employing is short for service life, and in the environment humidity bigger time
Wait, the most malfunctioning, it is impossible to well to play its effect.Therefore, need badly and find the one can be sensitive to hydrone, again on a large scale
Can monitor and separate the material of measured target gas station in time.
Metal-organic framework materials (MOFs) is the bonding mode and by coordinate bond by metal ion or metal cluster
A little organic ligands combine formation, due to metal ion or the difference of organic ligand, can show various topological structures.
MOFs self has that pore size is adjustable, specific surface area advantages of higher, and it is at gas-liquid separation, catalysis, optical, electrical, gas sensing etc.
Aspect has potential using value.Wherein HKUST-1 is a kind of typical metal-organic framework materials, and it is the quickest to hydrogen
Sense, when it contacts with hydrogen, the skeleton flexibility of HKUST-1 can become owing to sucking different guest molecules in duct
Changing, this change can cause again the change of its unit cell, and the change of unit cell eventually results in the change of HKUST-1 membrane resistance, logical
Cross and measure the concentration change reacting hydrogen to be measured that resistance can be sensitive.
The present invention, based on resistor-type HKUST-1 membrane material, designs hydrogen gas sensor, uses Cr film as the fork of sensitive blocks
Referring to electrode layer, Ni film is as the catalyst of HKUST-1 film forming.
The invention will be further described with the following Examples.
Application scenarios 1
Fig. 1 is the structural representation according to the waste old microwave automatic cracking reaction device shown in an exemplary embodiment
Figure, as it is shown in figure 1, include device body 8 and frequency conversion motor 19；Described frequency conversion motor 19 is connected with the rotary shaft of device body 8；
Described rotary shaft runs through described device body 8 and the axial direction along described device body 8 extends；With described frequency conversion motor 19 even
Connect and in the described rotary shaft of side, be provided with rotation shaft seal 18；Described rotary shaft is provided around matched spiral and pushes away
Enter device 22；Described rotary shaft side is provided with microwave magnetron 14；The shell side of described device body 8 is disposed with first
Manhole 9, cracking gas floss hole the 11, second manhole 12 and rubber raw materials entrance 13, opposite side be provided with for its
The connecting tube 23 that his cracking reaction device connects；Described cracking gas floss hole 11 is installed with detector 21.
The cracking reaction apparatus structure that the above embodiment of the present invention provides arranges rationally, further reduces cracking dress
The volume put, thus solve above-mentioned technical problem.
Preferably, the setting height(from bottom) of described microwave magnetron 14 matches with described spiral propeller 22.
Preferably, described detector 21 is installed in the lower section of described cracking gas floss hole 11 by fixture.
Preferably, described fixture is bolt.
Fig. 2 is the structural representation of the detector 21 used according to the present invention shown in an exemplary embodiment.As
Shown in Fig. 2, described detector 21 includes sensitive blocks 10 and data read module 20, during described sensitive blocks 10 is placed on
In the hollow structure shell with air-vent.
The structural representation of the sensitive blocks that Fig. 3 uses according to the present invention shown in an exemplary embodiment, such as Fig. 3 institute
Showing, this sensitive blocks 10 includes silicon chip substrate, PANI film 4, Ni film 5, HKUST-1 film 6 and BSP film 7；Described silicon chip substrate includes
Silicon chip 1, silicon nitride film 2 and Cr film layer 3, silicon nitride film 2 is used as insulating barrier, and Cr film layer 3 is used as interdigital electrode layer；Described Ni film 5
Prepared by employing magnetron sputtering method, thickness is 10nm；The thickness of described HKUST-1 film 6 is about 2～60 μm；Described Cr film layer 3 and number
It is conductively connected according to read module 20.
Fig. 4 is the preparation technology FB(flow block) of the sensitive blocks used according to the present invention shown in an exemplary embodiment,
As shown in Figure 4, the making of described sensitive blocks 10 comprises the steps:
Step one, preparation silicon chip substrate:
Take N-type silicon chip, cutting a size of 5cm × 1cm, sequentially pass through acetone, ethanol, deionized water ultrasonic cleaning, ultrasonic
Time is 30min, then dries up by nitrogen gun；Cleaned silicon chip is put into PECVD device, deposits one layer of silicon nitride film,
Thickness about 200nm；By Wafer Cleaning, spin coating one layer photoetching glue, photoresist parameter is low speed 900rpm spin coating 13s, at a high speed
4500rpm spin coating 50s；Being then covered by interdigital electrode mask, expose 7s, develop 65s；Putting in magnetic control sputtering device, magnetic control spatters
Penetrating Cr film, as interdigital electrode layer, thickness is 500nm, washes silicon chip surface photoresist subsequently；
Step 2, prepares microcavity:
The silicon chip substrate that will process through step one, first with 75% ethanol solution, its surface wipes is clean, use flame to add
Full-boiled process, is placed in silicon chip substrate on flame, from the beginning of one end, draws once at interval of 1cm, to form the microcavity of 2 tapers；Micro-
Cavity configuration enhances the sensitivity of sensitive blocks, and then the power of test of this detection equipment is strengthened so that it is the suction to hydrogen
Attached very competent；
Step 3, preparation PANI film:
Take a certain amount of polyaniline and be dissolved in dimethylformamide formation saturated solution, use spin coating-czochralski method to satisfy
With the surface that solution is spun to the silicon chip substrate processed through step 2, the speed of spin coating is 3000rpm, and then spin coating 10s exists
The baking oven of 100 DEG C is dried overnight, obtains PANI film on silicon chip substrate surface；
The type gas sense module used is due to based on resistive type metal-organic framework materials, and metal-organic framework materials
Film forming, on polyaniline film, owing to polyaniline has strong electric conductivity, therefore, further enhancing the spirit of type gas sense module
Sensitivity, and then make this detection equipment that the sensitivity of gas significantly to be strengthened；
Step 4, preparation HKUST-1 film:
1) putting in magnetron sputtering by silicon chip substrate, base vacuum is less than 1.5 × 10-3The Ni film of Pa, magnetron sputtering 10nm
5, silicon chip extracting is stand-by；
2) H is weighed3BTC 0.336g in another small beaker, with 19.2mL ethanol be completely dissolved water white transparency is molten
Liquid, weighs Cu (NO3)2·3H2O 0.7g, in small beaker, uses 19.2mL deionized water dissolving, by H3BTC solution is along walls of beaker
Pour Cu (NO into3)2·3H2O solution stirs half an hour, obtains HKUST-1 mother solution azury；The HKUST-1 mother that will prepare
Liquid and silicon chip substrate are placed in the reactor of 50mL, utilize hydrothermal synthesis method to synthesize MOF film, and reaction temperature is 135 DEG C, reacts 2
After it, repeatedly rinse several times with methanol after silicon chip substrate being taken out with tweezers, dry 1 hour in 100 DEG C, in silicon chip substrate
To blue HKUST-1 film, the thickness of HKUST-1 film is about 2～60 μm；
Owing to using Ni layer as the catalyst of metal-organic framework materials film forming, the Ni film meeting on PANI surface and HKUST-
1 film reaction, therefore, on the one hand promotes the film forming of HKUST-1, on the other hand improves the combination of PANI film and HKUST-1 film
Performance, makes to combine film layer and has higher stability, so that the sensing performance of the type gas sense module being thus prepared from
More stable；
Step 5, preparation BSP film:
1) BSP sub-micrometer rod growth: In (NO3)3·x H2O (0.08g) and H3BTC (0.068g) joins mixed solvent
H2In O/DMF (1:1,10mL), stir 10min under room temperature and make solution A, by photochromic compounds BSP
(0.057mmol) joining in solution A, dark place is stirred 1 hour；
2) film forming: by film forming on BSP solution rotation silicon chip/PANI/HKUST-1 film, the speed of rotation is 5000rpm, rotation
Time is 5 seconds；
Owing to, in the preparation process of the gas sensitization module used at it, adding on its surface and there is fluorescence property
BSP photochromic molecule, this photochromic molecule, under electromagnetism excitation, can send fluorescence in there is inflammable and explosive hazardous environment, make this
Detection equipment is capable of qualitative and quantitative detection environment and includes that hydrogen, at interior flammable explosive gas, can make to cause danger
The probability of situation reduces；
Step 5, sensitive blocks assembles:
Silicon chip substrate being put in hollow structure shell, wafer sections down, place towards small ventilating holes by sensitive thin film part,
Metal wire connects interdigital electrode and data read module on silicon chip.Owing to the manufacturing process of this sensitive blocks is the most simple and convenient and
Fast, substantial amounts of man power and material can be saved, there are the potentiality of large-scale industrial production.
Experiment test:
(1) experiments Hydrogen: 25 ± 2 DEG C of conditions, each leads into the nitrogen of air, hydrogen and hydrogen, and flow velocity is 1000ml/
Min, load resistance is 200 Ω；During blowing air, gas sensor signal value is O；It is passed through 1ppm hydrogen, gas sensor signal
Value changes to rapidly 1.0mV in 10s, and signal value tends towards stability in 20s；Being passed through air after 1min, signal value is in 5s
Return to 0 value and tend towards stability in 30s；Through 2000 stability tests, its data variation rate is less than 10%；Test result shows
Show that this solid waste analyte detection equipment has good response performance to hydrogen.
(2) ammonia experiment: 25 ± 2 DEG C of conditions, each leads into air ammonia and the nitrogen containing ammonia, and flow velocity is 1000ml/
Min, load resistance is 200 Ω；During blowing air, gas sensor signal value is O；Being passed through 100ppm ammonia, gas sensor is believed
Number value changes to rapidly 5.0mV in 10s, and signal value tends towards stability in 1min；Be passed through air after 5min, signal value in
Return to 0 value in 10s and tend towards stability in 0.5min；Through 2000 stability tests, its data variation rate is less than 10%；Survey
Test result shows that this solid waste analyte detection equipment has good response performance to ammonia.
(3) hydrogen sulfide experiment: 25 ± 2 DEG C of conditions, each leads into air and hydrogen sulfide containing nitrogen, and flow velocity is 1000ml/
Min, load resistance is 200 Ω；During blowing air, gas sensor signal value is O；Being passed through 0.05ppm hydrogen sulfide gas, gas passes
Sensor signal value changes to rapidly 3.0mV in 10s, and signal value tends towards stability in 30s；Air, signal it is passed through after 5min
It is worth and in 5s, returns to 0 value and tend towards stability in 10s；Through 2000 stability tests, its data variation rate is less than 10%；Survey
Test result shows that this solid waste analyte detection equipment has good response performance to hydrogen sulfide gas.
Test result indicate that: also this to ammonia and hydrogen sulfide poisonous and hazardous gas of this sensitive blocks has the strongest quick
Sense and selection performance, make this detection equipment all be improved sensitivity and the selectivity of toxic and harmful, reduce production
Risk.
Application scenarios 2
Fig. 1 is the structural representation according to the waste old microwave automatic cracking reaction device shown in an exemplary embodiment
Figure, as it is shown in figure 1, include device body 8 and frequency conversion motor 19；Described frequency conversion motor 19 is connected with the rotary shaft of device body 8；
Described rotary shaft runs through described device body 8 and the axial direction along described device body 8 extends；With described frequency conversion motor 19 even
Connect and in the described rotary shaft of side, be provided with rotation shaft seal 18；Described rotary shaft is provided around matched spiral and pushes away
Enter device 22；Described rotary shaft side is provided with microwave magnetron 14；The shell side of described device body 8 is disposed with first
Manhole 9, cracking gas floss hole the 11, second manhole 12 and rubber raw materials entrance 13, opposite side be provided with for its
The connecting tube 23 that his cracking reaction device connects；Described cracking gas floss hole 11 is installed with detector 21.
The cracking reaction apparatus structure that the above embodiment of the present invention provides arranges rationally, further reduces cracking dress
The volume put, thus solve above-mentioned technical problem.
Preferably, the setting height(from bottom) of described microwave magnetron 14 matches with described spiral propeller 22.
Preferably, described detector 21 is installed in the lower section of described cracking gas floss hole 11 by fixture.
Preferably, described fixture is bolt.
Fig. 2 is the structural representation of the detector 21 used according to the present invention shown in an exemplary embodiment.As
Shown in Fig. 2, described detector 21 includes sensitive blocks 10 and data read module 20, during described sensitive blocks 10 is placed on
In the hollow structure shell with air-vent.
Fig. 3 is the structural representation of the sensitive blocks used according to the present invention shown in an exemplary embodiment, such as Fig. 3 institute
Showing, this sensitive blocks 10 includes silicon chip substrate, PANI film 4, Ni film 5, HKUST-1 film 6 and BSP film 7；Described silicon chip substrate includes
Silicon chip 1, silicon nitride film 2 and Cr film layer 3, silicon nitride film 2 is used as insulating barrier, and Cr film layer 3 is used as interdigital electrode layer；Described Ni film 5
Prepared by employing magnetron sputtering method, thickness is 8nm；The thickness of described HKUST-1 film 6 is about 10 μm；Described Cr film layer 3 is read with data
Delivery block 20 is conductively connected.
Fig. 4 is the preparation technology FB(flow block) of the sensitive blocks used according to the present invention shown in an exemplary embodiment,
As shown in Figure 4, the making of described sensitive blocks 10 comprises the steps:
Step one, preparation silicon chip substrate:
Take N-type silicon chip, cutting a size of 5cm × 1cm, sequentially pass through acetone, ethanol, deionized water ultrasonic cleaning, ultrasonic
Time is 30min, then dries up by nitrogen gun；Cleaned silicon chip is put into PECVD device, deposits one layer of silicon nitride film,
Thickness about 210nm；By Wafer Cleaning, spin coating one layer photoetching glue, photoresist parameter is low speed 900rpm spin coating 13s, at a high speed
4500rpm spin coating 50s；Being then covered by interdigital electrode mask, expose 7s, develop 65s；Putting in magnetic control sputtering device, magnetic control spatters
Penetrating Cr film, as interdigital electrode layer, thickness is 510nm, washes silicon chip surface photoresist subsequently；
Step 2, prepares microcavity:
The silicon chip substrate that will process through step one, first with 75% ethanol solution, its surface wipes is clean, use flame to add
Full-boiled process, is placed in silicon chip substrate on flame, from the beginning of one end, draws once at interval of 1cm, to form the microcavity of 2 tapers；Micro-
Cavity configuration enhances the sensitivity of sensitive blocks, and then the power of test of this detection equipment is strengthened so that it is the suction to hydrogen
Attached very competent；
Step 3, preparation PANI film:
Take a certain amount of polyaniline and be dissolved in dimethylformamide formation saturated solution, use spin coating-czochralski method to satisfy
With the surface that solution is spun to the silicon chip substrate processed through step 2, the speed of spin coating is 3000rpm, and then spin coating 10s exists
The baking oven of 100 DEG C is dried overnight, obtains PANI film on silicon chip substrate surface；Step 4, preparation HKUST-1 film:
1) putting in magnetron sputtering by silicon chip substrate, base vacuum is less than 1.5 × 10-3The Ni film 5 of Pa, magnetron sputtering 8nm,
Silicon chip extracting is stand-by；
2) H is weighed3BTC 0.336g in another small beaker, with 19.2mL ethanol be completely dissolved water white transparency is molten
Liquid, weighs Cu (NO3)2·3H2O 0.7g, in small beaker, uses 19.2mL deionized water dissolving, by H3BTC solution is along walls of beaker
Pour Cu (NO into3)2·3H2O solution stirs half an hour, obtains HKUST-1 mother solution azury；The HKUST-1 mother that will prepare
Liquid and silicon chip substrate are placed in the reactor of 50mL, utilize hydrothermal synthesis method to synthesize MOF film, and reaction temperature is 135 DEG C, reacts 2
After it, repeatedly rinse several times with methanol after silicon chip substrate being taken out with tweezers, dry 1 hour in 100 DEG C, in silicon chip substrate
To blue HKUST-1 film, the thickness of HKUST-1 film is about 2～60 μm；Owing to using Ni layer as metal-organic framework materials
The catalyst of film forming, the Ni film on PANI surface can be with HKUST-1 film reaction, and therefore, on the one hand the rate of film build of HKUST-1 improves
10%, on the other hand PANI film improves 5% with the binding ability of HKUST-1 film, makes to combine film layer and has higher stability,
So that the sensing performance of the type gas sense module being thus prepared from is more stable；
Step 5, preparation BSP film:
1) BSP sub-micrometer rod growth: In (NO3)3·x H2O (0.08g) and H3BTC (0.068g) joins mixed solvent
H2In O/DMF (1:1,10mL), stir 10min under room temperature and make solution A, by photochromic compounds BSP
(0.057mmol) joining in solution A, dark place is stirred 1 hour；
2) film forming: by film forming on BSP solution rotation silicon chip/PANI/HKUST-1 film, the speed of rotation is 5000rpm, rotation
Time is 5 seconds；
Owing to, in the preparation process of the gas sensitization module used at it, adding on its surface and there is fluorescence property
BSP photochromic molecule, this photochromic molecule, under electromagnetism excitation, can send fluorescence in there is inflammable and explosive hazardous environment, make this
Detection equipment is capable of qualitative and quantitative detection environment and includes that hydrogen, at interior flammable explosive gas, can make to cause danger
The probability of situation reduces 10%；
Step 5, sensitive blocks assembles:
Silicon chip substrate being put in hollow structure shell, wafer sections down, place towards small ventilating holes by sensitive thin film part,
Metal wire connects interdigital electrode and data read module on silicon chip.Owing to the manufacturing process of this sensitive blocks is the most simple and convenient and
Fast, substantial amounts of man power and material can be saved, there are the potentiality of large-scale industrial production.
Experiment test:
(1) hydrogen test: 25 ± 2 DEG C of conditions, each leads into the nitrogen of air and hydrogen, and flow velocity is 1000ml/min,
Load resistance is 200 Ω；During blowing air, gas sensor signal value is O；Being passed through 10ppm hydrogen, gas sensor signal value exists
Change to rapidly 3.0mV in 8s, and signal value tends towards stability in 30s；Being passed through air after 1min, signal value returns to 0 in 10s
Value also tends towards stability in 1min；Through 2000 stability tests, its data variation rate is less than 10%.Test result shows this
Solid waste analyte detection equipment has good response performance to hydrogen.
(2) ammonia test: 25 ± 2 DEG C of conditions, each leads into air ammonia and the nitrogen containing ammonia, and flow velocity is 1000ml/
Min, load resistance is 200 Ω；During blowing air, gas sensor signal value is O；Being passed through 200ppm ammonia, gas sensor is believed
Number value changes to rapidly 10.0mV in 5s, and signal value tends towards stability in 1min；Be passed through air after 5min, signal value in
Return to 0 value in 10s and tend towards stability in 0.5min；Through 2000 stability tests, its data variation rate is less than 10%.Survey
Test result shows that this solid waste analyte detection equipment has good response performance to ammonia.
(3) hydrogen sulfide test: 25 ± 2 DEG C of conditions, each leads into air and hydrogen sulfide containing nitrogen, and flow velocity is 1000ml/
Min, load resistance is 200 Ω；During blowing air, gas sensor signal value is O；Being passed through 0.1ppm ammonia, gas sensor is believed
Number value changes to rapidly 5.0mV in 7s, and signal value tends towards stability in 30s；Being passed through air after 5min, signal value is in 5s
Return to 0 value and tend towards stability in 0.5min；Through 2000 stability tests, its data variation rate is less than 10%.Test knot
Fruit shows that this solid waste analyte detection equipment has good response performance to hydrogen sulfide gas.
Test result indicate that: the sensitive property of also this to ammonia and hydrogen sulfide poisonous and hazardous gas of this sensitive blocks increases
Strong 5% and select performance to improve 8%, make this detection equipment that sensitivity and the selectivity of toxic and harmful all to be carried
Height, reduces the risk of production.
Application scenarios 3
Fig. 1 is the structural representation according to the waste old microwave automatic cracking reaction device shown in an exemplary embodiment
Figure, as it is shown in figure 1, include device body 8 and frequency conversion motor 19；Described frequency conversion motor 19 is connected with the rotary shaft of device body 8；
Described rotary shaft runs through described device body 8 and the axial direction along described device body 8 extends；With described frequency conversion motor 19 even
Connect and in the described rotary shaft of side, be provided with rotation shaft seal 18；Described rotary shaft is provided around matched spiral and pushes away
Enter device 22；Described rotary shaft side is provided with microwave magnetron 14；The shell side of described device body 8 is disposed with first
Manhole 9, cracking gas floss hole the 11, second manhole 12 and rubber raw materials entrance 13, opposite side be provided with for its
The connecting tube 23 that his cracking reaction device connects；Described cracking gas floss hole 11 is installed with detector 21.
The cracking reaction apparatus structure that the above embodiment of the present invention provides arranges rationally, further reduces cracking dress
The volume put, thus solve above-mentioned technical problem.
Preferably, the setting height(from bottom) of described microwave magnetron 14 matches with described spiral propeller 22.
Preferably, described detector 21 is installed in the lower section of described cracking gas floss hole 11 by fixture.
Preferably, described fixture is bolt.
Fig. 2 is the structural representation of the detector 21 used according to the present invention shown in an exemplary embodiment.As
Shown in Fig. 2, described detector 21 includes sensitive blocks 10 and data read module 20, during described sensitive blocks 10 is placed on
In the hollow structure shell with air-vent.
Fig. 3 is the structural representation of the sensitive blocks used according to the present invention shown in an exemplary embodiment, such as Fig. 3 institute
Showing, this sensitive blocks 10 includes silicon chip substrate, PANI film 4, Ni film 5, HKUST-1 film 6 and BSP film 7；Described silicon chip substrate includes
Silicon chip 1, silicon nitride film 2 and Cr film layer 3, silicon nitride film 2 is used as insulating barrier, and Cr film layer 3 is used as interdigital electrode layer；Described Ni film 5
Prepared by employing magnetron sputtering method, thickness is 12nm；The thickness of described HKUST-1 film 6 is about 20 μm；Described Cr film layer 3 and data
Read module 20 is conductively connected.
Fig. 4 is the preparation technology FB(flow block) of the sensitive blocks used according to the present invention shown in an exemplary embodiment,
As shown in Figure 4, the making of described sensitive blocks 10 comprises the steps:
Step one, preparation silicon chip substrate:
Take N-type silicon chip, cutting a size of 5cm × 1cm, sequentially pass through acetone, ethanol, deionized water ultrasonic cleaning, ultrasonic
Time is 30min, then dries up by nitrogen gun；Cleaned silicon chip is put into PECVD device, deposits one layer of silicon nitride film,
Thickness about 220nm；By Wafer Cleaning, spin coating one layer photoetching glue, photoresist parameter is low speed 900rpm spin coating 13s, at a high speed
4500rpm spin coating 50s；Being then covered by interdigital electrode mask, expose 7s, develop 65s；Putting in magnetic control sputtering device, magnetic control spatters
Penetrating Cr film, as interdigital electrode layer, thickness is 550nm, washes silicon chip surface photoresist subsequently；
Step 2, prepares microcavity:
The silicon chip substrate that will process through step one, first with 75% ethanol solution, its surface wipes is clean, use flame to add
Full-boiled process, is placed in silicon chip substrate on flame, from the beginning of one end, draws once at interval of 1cm, to form the microcavity of 2 tapers；Micro-
Cavity configuration enhances the sensitivity of sensitive blocks, and then the power of test of this detection equipment is strengthened so that it is the suction to hydrogen
Attached very competent；
Step 3, preparation PANI film:
Take a certain amount of polyaniline and be dissolved in dimethylformamide formation saturated solution, use spin coating-czochralski method to satisfy
With the surface that solution is spun to the silicon chip substrate processed through step 2, the speed of spin coating is 3000rpm, and then spin coating 10s exists
The baking oven of 100 DEG C is dried overnight, obtains PANI film on silicon chip substrate surface；Step 4, preparation HKUST-1 film:
1) putting in magnetron sputtering by silicon chip substrate, base vacuum is less than 1.5 × 10-3The Ni film of Pa, magnetron sputtering 12nm
5, silicon chip extracting is stand-by；
Owing to using Ni layer as the catalyst of metal-organic framework materials film forming, the Ni film meeting on PANI surface and HKUST-
1 film reaction, therefore, on the one hand the rate of film build of HKUST-1 improves 20%, on the other hand PANI film and the combination of HKUST-1 film
Performance improves 10%, makes to combine film layer and has higher stability, so that the type gas sense module being thus prepared from
Sensing performance more stable；
2) H is weighed3BTC 0.336g in another small beaker, with 19.2mL ethanol be completely dissolved water white transparency is molten
Liquid, weighs Cu (NO3)2·3H2O 0.7g, in small beaker, uses 19.2mL deionized water dissolving, by H3BTC solution is along walls of beaker
Pour Cu (NO into3)2·3H2O solution stirs half an hour, obtains HKUST-1 mother solution azury；The HKUST-1 mother that will prepare
Liquid and silicon chip substrate are placed in the reactor of 50mL, utilize hydrothermal synthesis method to synthesize MOF film, and reaction temperature is 135 DEG C, reacts 2
After it, repeatedly rinse several times with methanol after silicon chip substrate being taken out with tweezers, dry 1 hour in 100 DEG C, in silicon chip substrate
To blue HKUST-1 film, the thickness of HKUST-1 film is about 2～60 μm；
Step 5, preparation BSP film:
1) BSP sub-micrometer rod growth: In (NO3)3·x H2O (0.08g) and H3BTC (0.068g) joins mixed solvent
H2In O/DMF (1:1,10mL), stir 10min under room temperature and make solution A, by photochromic compounds BSP
(0.057mmol) joining in solution A, dark place is stirred 1 hour；
2) film forming: by film forming on BSP solution rotation silicon chip/PANI/HKUST-1 film, the speed of rotation is 5000rpm, rotation
Time is 5 seconds；Owing to, in the preparation process of the gas sensitization module used at it, adding on its surface and there is fluorescence property
BSP photochromic molecule, this photochromic molecule, under electromagnetism excitation, can send fluorescence in there is inflammable and explosive hazardous environment, make
This detection equipment is capable of qualitative and quantitative detection environment and includes that hydrogen, at interior flammable explosive gas, can make to endanger
The probability of dangerous situation condition reduces 15%；
Step 5, sensitive blocks assembles:
Silicon chip substrate being put in hollow structure shell, wafer sections down, place towards small ventilating holes by sensitive thin film part,
Metal wire connects interdigital electrode and data read module on silicon chip.Owing to the manufacturing process of this sensitive blocks is the most simple and convenient and
Fast, substantial amounts of man power and material can be saved, there are the potentiality of large-scale industrial production.
Experiment test:
(1) hydrogen test: 25 ± 2 DEG C of conditions, each leads into the nitrogen of air, hydrogen and hydrogen, and flow velocity is 1000ml/
Min, load resistance is 200 Ω；During blowing air, gas sensor signal value is O；It is passed through 50ppm hydrogen, gas sensor signal
Value changes to rapidly 10.0mV in 5s, and signal value tends towards stability in 1min；Being passed through air after 5min, signal value is in 40s
Inside return to 0 value and tend towards stability in 1min；Through 2000 stability tests, its data variation rate is less than 10%.Test knot
Fruit shows that this solid waste analyte detection equipment has good response performance to hydrogen.
(2) ammonia test: 25 ± 2 DEG C of conditions, each leads into air ammonia and the nitrogen containing ammonia, and flow velocity is 1000ml/
Min, load resistance is 200 Ω；During blowing air, gas sensor signal value is O；Being passed through 500ppm ammonia, gas sensor is believed
Number value changes to rapidly 15.0mV in 2s, and signal value tends towards stability in 1min；Be passed through air after 5min, signal value in
Return to 0 value in 10s and tend towards stability in 1.5min；Through 2000 stability tests, its data variation rate is less than 10%.Survey
Test result shows that this solid waste analyte detection equipment has good response performance to ammonia.
(3) hydrogen sulfide test: 25 ± 2 DEG C of conditions, each leads into air and hydrogen sulfide containing nitrogen, and flow velocity is 1000ml/
Min, load resistance is 200 Ω；During blowing air, gas sensor signal value is O；It is passed through 1ppm ammonia, gas sensor signal
Value changes to rapidly 20.0mV in 3s, and signal value tends towards stability in 1min；Being passed through air after 5min, signal value is in 10s
Inside return to 0 value and tend towards stability in 1min；Through 2000 stability tests, its data variation rate is less than 10%.Test knot
Fruit shows that this solid waste analyte detection equipment has good response performance to hydrogen sulfide gas.
Test result indicate that: the sensitive property of also this to ammonia and hydrogen sulfide poisonous and hazardous gas of this sensitive blocks increases
Strong 10% and select performance to improve 16%, make this detection equipment that sensitivity and the selectivity of toxic and harmful all to be obtained
Improve, reduce the risk of production.
Application scenarios 4
Fig. 1 is the structural representation according to the waste old microwave automatic cracking reaction device shown in an exemplary embodiment
Figure, as it is shown in figure 1, include device body 8 and frequency conversion motor 19；Described frequency conversion motor 19 is connected with the rotary shaft of device body 8；
Described rotary shaft runs through described device body 8 and the axial direction along described device body 8 extends；With described frequency conversion motor 19 even
Connect and in the described rotary shaft of side, be provided with rotation shaft seal 18；Described rotary shaft is provided around matched spiral and pushes away
Enter device 22；Described rotary shaft side is provided with microwave magnetron 14；The shell side of described device body 8 is disposed with first
Manhole 9, cracking gas floss hole the 11, second manhole 12 and rubber raw materials entrance 13, opposite side be provided with for its
The connecting tube 23 that his cracking reaction device connects；Described cracking gas floss hole 11 is installed with detector 21.
The cracking reaction apparatus structure that the above embodiment of the present invention provides arranges rationally, further reduces cracking dress
The volume put, thus solve above-mentioned technical problem.
Preferably, the setting height(from bottom) of described microwave magnetron 14 matches with described spiral propeller 22.
Preferably, described detector 21 is installed in the lower section of described cracking gas floss hole 11 by fixture.
Preferably, described fixture is bolt.
Fig. 2 is the structural representation of the detector 21 used according to the present invention shown in an exemplary embodiment.As
Shown in Fig. 2, described detector 21 includes sensitive blocks 10 and data read module 20, during described sensitive blocks 10 is placed on
In the hollow structure shell with air-vent.
Fig. 3 is the structural representation of the sensitive blocks used according to the present invention shown in an exemplary embodiment, such as Fig. 3 institute
Showing, this sensitive blocks 10 includes silicon chip substrate, PANI film 4, Ni film 5, HKUST-1 film 6 and BSP film 7；Described silicon chip substrate includes
Silicon chip 1, silicon nitride film 2 and Cr film layer 3, silicon nitride film 2 is used as insulating barrier, and Cr film layer 3 is used as interdigital electrode layer；Described Ni film 5
Prepared by employing magnetron sputtering method, thickness is 20nm；The thickness of described HKUST-1 film 6 is about 40 μm；Described Cr film layer 3 and data
Read module 20 is conductively connected.
Fig. 4 is the preparation technology FB(flow block) of the sensitive blocks used according to the present invention shown in an exemplary embodiment,
As shown in Figure 4, the making of described sensitive blocks 10 comprises the steps:
Step one, preparation silicon chip substrate:
Take N-type silicon chip, cutting a size of 5cm × 1cm, sequentially pass through acetone, ethanol, deionized water ultrasonic cleaning, ultrasonic
Time is 30min, then dries up by nitrogen gun；Cleaned silicon chip is put into PECVD device, deposits one layer of silicon nitride film,
Thickness about 300nm；By Wafer Cleaning, spin coating one layer photoetching glue, photoresist parameter is low speed 900rpm spin coating 13s, at a high speed
4500rpm spin coating 50s；Being then covered by interdigital electrode mask, expose 7s, develop 65s；Putting in magnetic control sputtering device, magnetic control spatters
Penetrating Cr film, as interdigital electrode layer, thickness is 600nm, washes silicon chip surface photoresist subsequently；
Step 2, prepares microcavity:
The silicon chip substrate that will process through step one, first with 75% ethanol solution, its surface wipes is clean, use flame to add
Full-boiled process, is placed in silicon chip substrate on flame, from the beginning of one end, draws once at interval of 1cm, to form the microcavity of 2 tapers；Micro-
Cavity configuration enhances the sensitivity of sensitive blocks, and then the power of test of this detection equipment is strengthened so that it is the suction to hydrogen
Attached very competent；
Step 3, preparation PANI film:
Take a certain amount of polyaniline and be dissolved in dimethylformamide formation saturated solution, use spin coating-czochralski method to satisfy
With the surface that solution is spun to the silicon chip substrate processed through step 2, the speed of spin coating is 3000rpm, and then spin coating 10s exists
The baking oven of 100 DEG C is dried overnight, obtains PANI film on silicon chip substrate surface；Step 4, preparation HKUST-1 film:
1) putting in magnetron sputtering by silicon chip substrate, base vacuum is less than 1.5 × 10-3The Ni film of Pa, magnetron sputtering 10nm
5, silicon chip extracting is stand-by；Owing to using Ni layer as the catalyst of metal-organic framework materials film forming, the Ni film meeting on PANI surface
With HKUST-1 film reaction, therefore, on the one hand the rate of film build of HKUST-1 improves 30%, on the other hand PANI film and HKUST-1
The binding ability of film improves 20%, makes to combine film layer and has higher stability, so that the gas being thus prepared from
The sensing performance of sensing module is more stable；
2) H is weighed3BTC 0.336g in another small beaker, with 19.2mL ethanol be completely dissolved water white transparency is molten
Liquid, weighs Cu (NO3)2·3H2O 0.7g, in small beaker, uses 19.2mL deionized water dissolving, by H3BTC solution is along walls of beaker
Pour Cu (NO into3)2·3H2O solution stirs half an hour, obtains HKUST-1 mother solution azury；The HKUST-1 mother that will prepare
Liquid and silicon chip substrate are placed in the reactor of 50mL, utilize hydrothermal synthesis method to synthesize MOF film, and reaction temperature is 135 DEG C, reacts 2
After it, repeatedly rinse several times with methanol after silicon chip substrate being taken out with tweezers, dry 1 hour in 100 DEG C, in silicon chip substrate
To blue HKUST-1 film, the thickness of HKUST-1 film is about 2～60 μm；
Step 5, preparation BSP film:
1) BSP sub-micrometer rod growth: In (NO3)3·x H2O (0.08g) and H3BTC (0.068g) joins mixed solvent
H2In O/DMF (1:1,10mL), stir 10min under room temperature and make solution A, by photochromic compounds BSP
(0.057mmol) joining in solution A, dark place is stirred 1 hour；
2) film forming: by film forming on BSP solution rotation silicon chip/PANI/HKUST-1 film, the speed of rotation is 5000rpm, rotation
Time is 5 seconds；Owing to, in the preparation process of the gas sensitization module used at it, adding on its surface and there is fluorescence property
BSP photochromic molecule, this photochromic molecule, under electromagnetism excitation, can send fluorescence in there is inflammable and explosive hazardous environment, make
This detection equipment is capable of qualitative and quantitative detection environment and includes that hydrogen, at interior flammable explosive gas, can make to endanger
The probability of dangerous situation condition reduces 35%；
Step 5, sensitive blocks assembles:
Silicon chip substrate being put in hollow structure shell, wafer sections down, place towards small ventilating holes by sensitive thin film part,
Metal wire connects interdigital electrode and data read module on silicon chip.Owing to the manufacturing process of this sensitive blocks is the most simple and convenient and
Fast, substantial amounts of man power and material can be saved, there are the potentiality of large-scale industrial production.
Experiment test:
(1) hydrogen test: 25 ± 2 DEG C of conditions, each leads into the nitrogen of air, hydrogen and hydrogen, and flow velocity is 1000ml/
Min, load resistance is 200 Ω；During blowing air, gas sensor signal value is O；Being passed through 1 00ppm hydrogen, gas sensor is believed
Number value changes to rapidly 30.0mV in 3s, and signal value tends towards stability in 20s；Being passed through air after 5min, signal value is in 20s
Inside return to 0 value and tend towards stability in 2min；Through 2000 stability tests, its data variation rate is less than 10%.Test knot
Fruit shows that this solid waste analyte detection equipment has good response performance to hydrogen.
(2) ammonia test: 25 ± 2 DEG C of conditions, each leads into air ammonia and the nitrogen containing ammonia, and flow velocity is 1000ml/
Min, load resistance is 200 Ω；During blowing air, gas sensor signal value is O；It is passed through 1000ppm ammonia, sensor signal value
In 2s, change to rapidly 10.0mV, and signal value tends towards stability in 2min；Being passed through air after 5min, signal value is in 10s
Return to 0 value and tend towards stability in 2min；Through 2000 stability tests, its data variation rate is less than 10%.Test result
Show that this solid waste analyte detection equipment has good response performance to ammonia.
(3) hydrogen sulfide test: 25 ± 2 DEG C of conditions, each leads into air and hydrogen sulfide containing nitrogen, and flow velocity is 1000ml/
Min, load resistance is 200 Ω；During blowing air, gas sensor signal value is O；Being passed through 10ppm ammonia, sensor signal value exists
Change to rapidly 25.0mV in 2s, and signal value tends towards stability in 2min；Being passed through air after 5min, signal value returns in 40s
To 0 value and tend towards stability in 2min；Through 2000 stability tests, its data variation rate is less than 10%.Test result shows
Show that this solid waste analyte detection equipment has good response performance to hydrogen sulfide gas.
Test result indicate that: the sensitive property of also this to ammonia and hydrogen sulfide poisonous and hazardous gas of this sensitive blocks increases
Strong 20% and select performance to improve 30%, make this detection equipment that sensitivity and the selectivity of toxic and harmful all to be obtained
Improve, reduce the risk of production.
Application scenarios 5
Fig. 1 is the structural representation according to the waste old microwave automatic cracking reaction device shown in an exemplary embodiment
Figure, as it is shown in figure 1, include device body 8 and frequency conversion motor 19；Described frequency conversion motor 19 is connected with the rotary shaft of device body 8；
Described rotary shaft runs through described device body 8 and the axial direction along described device body 8 extends；With described frequency conversion motor 19 even
Connect and in the described rotary shaft of side, be provided with rotation shaft seal 18；Described rotary shaft is provided around matched spiral and pushes away
Enter device 22；Described rotary shaft side is provided with microwave magnetron 14；The shell side of described device body 8 is disposed with first
Manhole 9, cracking gas floss hole the 11, second manhole 12 and rubber raw materials entrance 13, opposite side be provided with for its
The connecting tube 23 that his cracking reaction device connects；Described cracking gas floss hole 11 is installed with detector 21.
The cracking reaction apparatus structure that the above embodiment of the present invention provides arranges rationally, further reduces cracking dress
The volume put, thus solve above-mentioned technical problem.
Preferably, the setting height(from bottom) of described microwave magnetron 14 matches with described spiral propeller 22.
Preferably, described detector 21 is installed in the lower section of described cracking gas floss hole 11 by fixture.
Preferably, described fixture is bolt.
Fig. 2 is the structural representation of the detector 21 used according to the present invention shown in an exemplary embodiment.As
Shown in Fig. 2, described detector 21 includes sensitive blocks 10 and data read module 20, during described sensitive blocks 10 is placed on
In the hollow structure shell with air-vent.
Fig. 3 is the structural representation of the sensitive blocks used according to the present invention shown in an exemplary embodiment, such as Fig. 3 institute
Showing, this sensitive blocks 10 includes silicon chip substrate, PANI film 4, Ni film 5, HKUST-1 film 6 and BSP film 7；Described silicon chip substrate includes
Silicon chip 1, silicon nitride film 2 and Cr film layer 3, silicon nitride film 2 is used as insulating barrier, and Cr film layer 3 is used as interdigital electrode layer；Described Ni film 5
Prepared by employing magnetron sputtering method, thickness is 30nm；The thickness of described HKUST-1 film 6 is about 60 μm；Described Cr film layer 3 and data
Read module 20 is conductively connected.
Fig. 4 is the preparation technology FB(flow block) of the sensitive blocks used according to the present invention shown in an exemplary embodiment,
As shown in Figure 4, the making of described sensitive blocks 10 comprises the steps:
Step one, preparation silicon chip substrate:
Take N-type silicon chip, cutting a size of 5cm × 1cm, sequentially pass through acetone, ethanol, deionized water ultrasonic cleaning, ultrasonic
Time is 30min, then dries up by nitrogen gun；Cleaned silicon chip is put into PECVD device, deposits one layer of silicon nitride film,
Thickness about 400nm；By Wafer Cleaning, spin coating one layer photoetching glue, photoresist parameter is low speed 900rpm spin coating 13s, at a high speed
4500rpm spin coating 50s；Being then covered by interdigital electrode mask, expose 7s, develop 65s；Putting in magnetic control sputtering device, magnetic control spatters
Penetrating Cr film, as interdigital electrode layer, thickness is 700nm, washes silicon chip surface photoresist subsequently；
Step 2, prepares microcavity:
The silicon chip substrate that will process through step one, first with 75% ethanol solution, its surface wipes is clean, use flame to add
Full-boiled process, is placed in silicon chip substrate on flame, from the beginning of one end, draws once at interval of 1cm, to form the microcavity of 2 tapers；Micro-
Cavity configuration enhances the sensitivity of sensitive blocks, and then the power of test of this detection equipment is strengthened so that it is the suction to hydrogen
Attached very competent；
Step 3, preparation PANI film:
Take a certain amount of polyaniline and be dissolved in dimethylformamide formation saturated solution, use spin coating-czochralski method to satisfy
With the surface that solution is spun to the silicon chip substrate processed through step 2, the speed of spin coating is 3000rpm, and then spin coating 10s exists
The baking oven of 100 DEG C is dried overnight, obtains PANI film on silicon chip substrate surface；Step 4, preparation HKUST-1 film:
1) putting in magnetron sputtering by silicon chip substrate, base vacuum is less than 1.5 × 10-3The Ni film of Pa, magnetron sputtering 30nm
5, silicon chip extracting is stand-by；
2) H is weighed3BTC 0.336g in another small beaker, with 19.2mL ethanol be completely dissolved water white transparency is molten
Liquid, weighs Cu (NO3)2·3H2O 0.7g, in small beaker, uses 19.2mL deionized water dissolving, by H3BTC solution is along walls of beaker
Pour Cu (NO into3)2·3H2O solution stirs half an hour, obtains HKUST-1 mother solution azury；The HKUST-1 mother that will prepare
Liquid and silicon chip substrate are placed in the reactor of 50mL, utilize hydrothermal synthesis method to synthesize MOF film, and reaction temperature is 135 DEG C, reacts 2
After it, repeatedly rinse several times with methanol after silicon chip substrate being taken out with tweezers, dry 1 hour in 100 DEG C, in silicon chip substrate
To blue HKUST-1 film, the thickness of HKUST-1 film is about 2～60 μm；Owing to using Ni layer as metal-organic framework materials
The catalyst of film forming, the Ni film on PANI surface can be with HKUST-1 film reaction, and therefore, on the one hand the rate of film build of HKUST-1 improves
30%, on the other hand PANI film improves 20% with the binding ability of HKUST-1 film, makes to combine film layer and has higher stablizing
Property, so that the sensing performance of the type gas sense module being thus prepared from is more stable；
Step 5, preparation BSP film:
1) BSP sub-micrometer rod growth: In (NO3)3·x H2O (0.08g) and H3BTC (0.068g) joins mixed solvent
H2In O/DMF (1:1,10mL), stir 10min under room temperature and make solution A, by photochromic compounds BSP
(0.057mmol) joining in solution A, dark place is stirred 1 hour；
2) film forming: by film forming on BSP solution rotation silicon chip/PANI/HKUST-1 film, the speed of rotation is 5000rpm, rotation
Time is 5 seconds；Owing to, in the preparation process of the gas sensitization module used at it, adding on its surface and there is fluorescence property
BSP photochromic molecule, this photochromic molecule, under electromagnetism excitation, can send fluorescence in there is inflammable and explosive hazardous environment, make
This detection equipment is capable of qualitative and quantitative detection environment and includes that hydrogen, at interior flammable explosive gas, can make to endanger
The probability of dangerous situation condition reduces 50%；
Step 5, sensitive blocks assembles:
Silicon chip substrate being put in hollow structure shell, wafer sections down, place towards small ventilating holes by sensitive thin film part,
Metal wire connects interdigital electrode and data read module on silicon chip.Owing to the manufacturing process of this sensitive blocks is the most simple and convenient and
Fast, substantial amounts of man power and material can be saved, there are the potentiality of large-scale industrial production.
Experiment test:
(1) hydrogen test: 25 ± 2 DEG C of conditions, each leads into the nitrogen of air, hydrogen and hydrogen, and flow velocity is 1000ml/
Min, load resistance is 200 Ω；During blowing air, gas sensor signal value is O；Being passed through 500ppm hydrogen, gas sensor is believed
Number value changes to rapidly 50.0mV in 2s, and signal value tends towards stability in 2min；Be passed through air after 5min, signal value in
Return to 0 value in 1min and tend towards stability in 2min；Through 2000 stability tests, its data variation rate is less than 10%.Survey
Test result shows that this solid waste analyte detection equipment has good response performance to hydrogen.
(2) ammonia test: 25 ± 2 DEG C of conditions, each leads into air ammonia and the nitrogen containing ammonia, and flow velocity is 1000ml/
Min, load resistance is 200 Ω；During blowing air, gas sensor signal value is O；Being passed through 2000ppm ammonia, gas is through 2000
Secondary stability test, sensor signal value changes to rapidly 15.0mV in 1s, and signal value tends towards stability in 2min；5min
After be passed through air, signal value returns to 0 value in 20s and tends towards stability in 5min；Its data variation rate is less than 10%.Pass through
2000 stability tests, its data variation rate is less than 10%.Test result shows that this solid waste analyte detection equipment is to ammonia
There is good response performance.
(3) hydrogen sulfide test: 25 ± 2 DEG C of conditions, each leads into air and hydrogen sulfide containing nitrogen, and flow velocity is 1000ml/
Min, load resistance is 200 Ω；During blowing air, gas sensor signal value is O；It is passed through 100ppm ammonia, sensor signal value
In 1s, change to rapidly 30.0mV, and signal value tends towards stability in 3min；Being passed through air after 5min, signal value is in 2min
Return to 0 value and tend towards stability in 5min；Its data variation rate is less than 10%.Through 2000 stability tests, its data become
Rate is less than 10%.Test result shows that this solid waste analyte detection equipment has good response performance to hydrogen sulfide gas.
Test result indicate that: the sensitive property of also this to ammonia and hydrogen sulfide poisonous and hazardous gas of this sensitive blocks increases
Strong by 40%, select performance to improve 50%, make this detection equipment that sensitivity and the selectivity of toxic and harmful all to be obtained
Improve, reduce the risk of production.
From the point of view of applicable cases according to application scenarios 1 to application scenarios 5, the waste old microwave that the present invention provides splits automatically
Solution reaction unit has the advantage that
1, the type gas sense module that the present invention uses is due to based on resistive type metal-organic framework materials, and metal is organic
Framework material film forming, on polyaniline film, owing to polyaniline has strong electric conductivity, therefore, further enhancing gas sensing
The sensitivity of module, and then make this detection equipment that the sensitivity of gas significantly to be strengthened.Additionally, due to use Ni
Layer is as the catalyst of metal-organic framework materials film forming, and the Ni film on PANI surface can be with HKUST-1 film reaction, therefore, and a side
Face promotes the film forming of HKUST-1, on the other hand improves the binding ability of PANI film and HKUST-1 film, makes to combine film layer tool
There is higher stability, so that the sensing performance of the type gas sense module being thus prepared from is more stable.
2, due to the fact that in the preparation process of its gas sensitization module used, add on its surface and there is fluorescence
The BSP photochromic molecule of performance, this photochromic molecule, under electromagnetism excitation, can send glimmering in there is inflammable and explosive hazardous environment
Light, makes this detection equipment be capable of qualitative and quantitative detection environment and includes that hydrogen, at interior flammable explosive gas, can make
The probability of situation of causing danger reduces.
3, the present invention use polyaniline as substrate liquid spin coating silicon chip substrate, owing to making silicon chip substrate system in preparation process
Having become the structure of similar microcavity, and added the material including BSP, micro-cavity structure enhances the sensitivity of sensitive blocks,
And then the power of test of this detection equipment is strengthened so that it is extremely strong to the absorbability of hydrogen；Additionally, this sensitive blocks is the most right
Ammonia and this poisonous and hazardous gas of hydrogen sulfide have the strongest sensitivity and select performance, make this detection equipment to poisonous and harmful
Sensitivity and the selectivity of gas are all improved, and reduce the risk of production；Finally, due to the manufacturing process of this sensitive blocks
The most simple and convenient and quick, substantial amounts of man power and material can be saved, there are the potentiality of large-scale industrial production, therefore, this Shen
The waste old microwave automatic cracking reaction device that embodiment please is provided has great promotional value.
Last it should be noted that, above example is only in order to illustrate technical scheme, rather than the present invention is protected
Protecting the restriction of scope, although having made to explain to the present invention with reference to preferred embodiment, those of ordinary skill in the art should
Work as understanding, technical scheme can be modified or equivalent, without deviating from the reality of technical solution of the present invention
Matter and scope.
Claims (4)
1. waste old microwave automatic cracking reaction device, it is characterised in that include device body and frequency conversion motor；Described frequency conversion
Motor is connected with the rotary shaft of device body；Described rotary shaft runs through described device body the axial side along described device body
To extension；It is connected in the described rotary shaft of side with described frequency conversion motor and is provided with rotation shaft seal；Around described rotary shaft
It is provided with matched spiral propeller；Described rotary shaft side is provided with microwave magnetron；The shell of described device body
Side is disposed with the first manhole, cracking gas floss hole, the second manhole and rubber raw materials entrance, and opposite side is arranged
There is the connecting tube for being connected with other cracking reaction devices；Described device body is fixedly provided with detector.
Waste old microwave the most according to claim 1 automatic cracking reaction device, it is characterised in that described microwave magnetic control
The setting height(from bottom) of pipe matches with described spiral propeller, and described detector is fixedly arranged on below cracking gas floss hole.
Waste old microwave the most according to claim 2 automatic cracking reaction device, it is characterised in that described gas detecting
Device is installed in the lower section of described cracking gas floss hole by fixture.
Waste old microwave the most according to claim 3 automatic cracking reaction device, it is characterised in that described fixture is
Bolt.
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| CN107376802A (en) * | 2017-09-15 | 2017-11-24 | 四川宏图普新微波科技有限公司 | The technique of clean operation in a kind of holding chamber for microwave cracking damaged tire |
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| CN102140362A (en) * | 2011-01-26 | 2011-08-03 | 刘建波 | Automatic microwave cracking reaction device for waste rubber |
| CN105717109A (en) * | 2016-04-21 | 2016-06-29 | 林业城 | Hydrogen gas sensor based on gasochromic function |
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2016
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102140362A (en) * | 2011-01-26 | 2011-08-03 | 刘建波 | Automatic microwave cracking reaction device for waste rubber |
| CN105717109A (en) * | 2016-04-21 | 2016-06-29 | 林业城 | Hydrogen gas sensor based on gasochromic function |
Cited By (2)
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| CN107376802A (en) * | 2017-09-15 | 2017-11-24 | 四川宏图普新微波科技有限公司 | The technique of clean operation in a kind of holding chamber for microwave cracking damaged tire |
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