CN104760972B - A kind of preparation method of same crystalline phase core shell structure beta-molecular sieve - Google Patents
A kind of preparation method of same crystalline phase core shell structure beta-molecular sieve Download PDFInfo
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Abstract
The present invention relates to the preparation method of a kind of same crystalline phase core shell structure beta-molecular sieve, it is with white carbon, tetraethyl orthosilicate, sodium metaaluminate, tetraethyl ammonium hydroxide, ammonium fluoride is raw material, the tetraethyl ammonium hydroxide aqueous solution is inorganic agent, first synthesis nuclear phase beta-molecular sieve, blended liquid is prepared, reactor crystallization, heated at constant temperature, quenching, clean dispersion, centrifugation, vacuum drying, high-temperature vacuum roasting, make same crystalline phase core shell structure beta-molecular sieve, this preparation method technique is advanced, data are the fullest and the most accurate, same crystalline phase core shell structure zeolite crystal diameter 15～20 μm of preparation, crystal grain outside nanocrystal parcel is closely, product parcel degree reaches 97%, product purity reaches 99.9%, can mate with multiple chemical substance and use as catalyst, it it is the preparation method of very good same crystalline phase core shell structure beta-molecular sieve.
Description
Technical field
The present invention relates to the preparation method of a kind of same crystalline phase core shell structure beta-molecular sieve, belong to zeolite multiple
Close catalysis material preparation and the technical field of application.
Background technology
Beta-molecular sieve has the topological structure of uniqueness, is that one has three-dimensional twelve-ring duct knot
The high-silica zeolite of structure, has good heat endurance, hydrophobicity, acid resistance, anti-coking,
Be widely used in being hydrocracked, hydrocarbon isomerization, alkylating aromatic hydrocarbon, purifying vehicle exhaust are urged
Change process.
In catalytic process, beta-molecular sieve area carbon is to cause one of its catalyst deactivation mainly
Reason, at present, along with the further investigation to nanometer technology, nano beta molecular sieve is bigger because of it
Specific surface area, shorter pore passage structure and more surface-active so that it is can well
Weaken even elimination carbon distribution problem, but there is also perhaps during preparing nano beta molecular sieve
Many shortcomings, oxidizable moisture absorption, easily reunion, poor stability；Micron order big crystal grain beta-molecular sieve can
With the diffusion path that offer is longer, catalytic reaction can be played regulation effect；Existing single knot
There is many drawbacks in the beta-molecular sieve of structure, constrains application industrially.
Summary of the invention
Goal of the invention
It is an object of the invention to the situation for background technology and deficiency, with white carbon, positive silicic acid
Ethyl ester, sodium metaaluminate are raw material, first prepare nuclear phase beta-molecular sieve, through static crystallization, quenching,
Separation, vacuum baking, make the same crystalline phase core shell structure beta-molecular sieve of band clad, with significantly
Degree improves the purity of core shell structure beta-molecular sieve, expands the range of application of beta-molecular sieve.
Technical scheme
The present invention use chemical substance material be: white carbon, tetraethyl orthosilicate, sodium metaaluminate,
Ammonium fluoride, tetraethyl ammonium hydroxide, deionized water, argon gas, its prepare consumption as follows: with gram,
Milliliter, centimetre3For measurement unit
White carbon: SiO2, 2g ± 0.001g
Tetraethyl orthosilicate: Si (OC2H5)4, 20.79mL ± 0.01mL
Sodium metaaluminate: NaAlO2, 0.171g ± 0.001g
Ammonium fluoride: NH4F, 1.891g ± 0.001g
Tetraethyl ammonium hydroxide: (C2H5)4NOH, concentration 25%, 80mL ± 0.01mL
Deionized water: H2O, 5000mL ± 50mL
Argon gas: Ar, 100000cm3±100cm3
Preparation method is as follows:
(1) configuration inorganic agent
Measure tetraethyl ammonium hydroxide 5.89mL ± 0.01mL, deionized water
24.11mL ± 0.01mL, adds in beaker, stirs 30min, become the tetrem of 0.341mol/L
Base ammonium hydroxide aqueous solution 30mL；
(2) nuclear phase beta-molecular sieve is prepared
1. preparation nuclear phase beta-molecular sieve mixed solution
Measure tetraethyl orthosilicate 20.79mL ± 0.01mL, deionized water 5mL ± 0.01mL, four
Ethyl ammonium hydroxide 28mL ± 0.01mL, weighs ammonium fluoride 1.891g ± 0.001g, adds beaker
In, it being stirred, mixing time 300min, the volatile materials making mixture produce is abundant
Volatilization, forms white gels mixed solution；
2. heating crystallization
The white gels mixed solution of preparation is moved in polytetrafluoroethylcontainer container, is subsequently placed in anti-
Answer in still, and airtight；
Reactor is placed in airtight heating in insulating box, heating-up temperature 150 DEG C ± 2 DEG C, constant temperature,
Insulation, static crystallization 120h, become crystallization gel solution；
3. quenching
After reaction terminates, close insulating box, take out reactor and be placed in quenching groove, at 10 DEG C
Deionized water in be quickly cooled to 20 DEG C；
4. centrifugation
Open reactor, take out polytetrafluoroethylcontainer container, by the crystallization in polytetrafluoroethylcontainer container
Gel solution is placed in centrifuge tube, is centrifuged separating, centrifugation revolution 5000r/min,
Disengaging time 20min, retains solid sediment, discards supernatant after centrifugation；
5. it is vacuum dried
Solid sediment is placed in evaporating dish, is subsequently placed in vacuum drying chamber and is dried, be dried
Temperature 120 DEG C, vacuum 10Pa, drying time 6h, dried nuclear phase beta-molecular sieve powder
End 6g ± 0.001g；
(3) pretreatment nuclear phase beta-molecular sieve
1. preparation pretreatment nuclear phase beta-molecular sieve solution
By nuclear phase beta-molecular sieve powder 5g ± 0.001g, the tetraethyl ammonium hydroxide aqueous solution
25mL ± 0.01mL, adds in polytetrafluoroethylcontainer container, is stirred vigorously 1h, obtains mixing molten
Liquid；
2. isothermal reaction
The polytetrafluoroethylcontainer container filling mixed solution is put in reactor and airtight, will reaction
Still is placed in insulating box heating, heating-up temperature 100 DEG C ± 2 DEG C, and constant temperature, insulation, static state are instead
Answer 24h；
3. quenching
Stop heating after reaction, reactor is moved in quenching groove, the deionized water of 10 DEG C
In be quickly cooled to 20 DEG C；
4. wash
Open reactor, the mixed solution in polytetrafluoroethylcontainer container is poured in beaker, add
Deionized water 500mL, agitator treating 10min, become cleaning solution；
5. centrifugation
Cleaning solution is placed in centrifuge tube, is centrifuged separating, centrifugation revolution 5000r/min,
Disengaging time 20min, after centrifugation, retains solid sediment, discards supernatant；
6. it is vacuum dried
Solid sediment is placed in evaporating dish, is subsequently placed in vacuum drying chamber and is dried, be dried
Temperature 120 DEG C, vacuum 10Pa, drying time 6h, the dried nuclear phase β that must pre-process
Molecular sieve powder 4.5g ± 0.001g；
(4) preparation is with crystalline phase core shell structure beta-molecular sieve
1. same crystalline phase core shell structure beta-molecular sieve mixed solution is prepared
Measure deionized water 3.1mL ± 0.01mL, tetraethyl ammonium hydroxide 11.52mL ± 0.01mL,
Weigh sodium metaaluminate 0.171g ± 0.001g, white carbon 2g ± 0.001g joins polytetrafluoroethylene (PTFE) and holds
In device, use heat collecting type constant temperature blender with magnetic force heated at constant temperature stirring 2h, heating-up temperature 80 DEG C
± 2 DEG C, agitation revolution 600r/min, make mixture fully dissolve, form clear gel solution；
In gel solution, add the nuclear phase beta-molecular sieve 4g ± 0.001g of pretreatment, continue stirring 30min,
Become mixed solution；
2. static crystallization is heated
The polytetrafluoroethylcontainer container filling mixed solution is placed in reactor, and airtight, then
Reactor is put in insulating box and heat, heating-up temperature 140 DEG C ± 2 DEG C, constant temperature, static crystalline substance
Change reaction 48h；
3. quenching
After crystallization, stop heating, open insulating box, take out reactor, be placed in quenching groove
In, the deionized water of 10 DEG C is quickly cooled to 20 DEG C；
4. deionized water dilution, centrifugation
Open reactor after cooling, the mixed solution in polytetrafluoroethylcontainer container poured in beaker,
Add deionized water 500mL, magnetic stirring apparatus stirs 30min, becomes dilution mixture solution；
Dilution mixture solution is placed in the centrifuge tube of centrifuge, is centrifuged separating, centrifugal point
From revolution 8000r/min, centrifugation time 30min, after centrifugation, retain sediment,
Discard supernatant；
5. dispersion, centrifugation are cleaned
Put the precipitate in beaker, add deionized water 500mL, be subsequently placed in ultrasonic wavelength-division
Dissipating in instrument, carry out ultrasonic cleaning and dispersion, ultrasonic frequency is 40KHz, jitter time 30min；
Then dispersion soln is placed in the centrifuge tube of centrifuge and is centrifuged separating, centrifugation
Revolution 8000r/min, centrifugation time 30min, retain sediment, abandon after centrifugation
Fall supernatant；
Clean dispersion, centrifugation repeats 3 times；
6. vacuum baking
Carry out in vacuum sintering furnace with the roasting of crystalline phase core shell structure beta-molecular sieve, be
Heat, vacuumize, argon shield, complete under outer water circulating cooling；
Put the precipitate in quartz container, be subsequently placed on the workbench in vacuum sintering furnace；
Closing vacuum sintering furnace, open vavuum pump, extract furnace air, in making stove, pressure reaches
5Pa；
Opening argon bottle, tunger tube, be passed through argon gas in stove, in making stove, invariablenes pressure of liquid exists
0.09MPa；
Open outer water circulating cooling pipe, carry out outer water circulating cooling；
Opening resistor heater, heating-up temperature 550 DEG C ± 2 DEG C, carry out roasting, add thermal bake-out
Time 300min；
Stopping heating after roasting, the product in quartz container cools to 25 DEG C with the furnace；
Must be with crystalline phase core shell structure beta-molecular sieve after cooling；
(5) detect, analyze, characterize
The crystal structure of same crystalline phase core shell structure beta-molecular sieve, the grain morphology of preparation is examined
Survey, analyze, characterize；
Crystalline product morphology analysis is carried out by SEM；
Crystalline product thing phase and crystallinity analysis is carried out with X-ray diffractometer；
Conclusion: be white powder with crystalline phase core shell structure beta-molecular sieve, powder granule diameter
15～20 μm, extra-granular is wrapped up by nanocrystal, and inside is micron grain, for core shell structure,
Product parcel degree reaches 97%, and product purity reaches 99.9%；
(6) store
The same crystalline phase core shell structure beta-molecular sieve white powder of preparation is put in valve bag and seals,
Valve bag is stored in the glass container of amber transparent, seals lucifuge and store, need protection against the tide, prevent
Shine, anti-acid-alkali salt class material corrodes, storage temperature 20 DEG C, relative humidity≤10%.
Beneficial effect
The present invention has obvious advance compared with background technology, is with white carbon, positive silicic acid
Ethyl ester, sodium metaaluminate, tetraethyl ammonium hydroxide, ammonium fluoride are raw material, with tetraethyl hydroxide
Aqueous ammonium is inorganic agent, with deionized water as solvent, washing agent, and first synthesis nuclear phase beta molecule
Sieve, then processes nuclear phase beta-molecular sieve with inorganic agent, is finally synthesizing same crystalline phase nucleocapsid knot
Structure beta-molecular sieve is the preparation of blended liquid, reactor crystallization, heated at constant temperature, quenching, clear
Wash dispersion, centrifugation, vacuum drying, high-temperature vacuum roasting, make same crystalline phase core shell structure
Beta-molecular sieve, this preparation method technique is advanced, and data are the fullest and the most accurate, the same crystalline phase nucleocapsid of preparation
Structure molecular screen crystal grain diameter 15～20 μm, crystal grain outside nanocrystal parcel is tight, product bag
Degree of wrapping up in reaches 97%, and product purity reaches 99.9%, can mate with multiple chemical substance and make catalyst and make
With, it is the very good preparation method with crystalline phase core shell structure beta-molecular sieve.
Accompanying drawing explanation
Fig. 1 is same crystalline phase core shell structure beta-molecular sieve vacuum baking state diagram
Fig. 2 is same crystalline phase core shell structure beta-molecular sieve shape appearance figure
Fig. 3 is same crystalline phase core shell structure beta-molecular sieve X-ray diffraction intensity spectrogram
Shown in figure, list of numerals is as follows:
1, vacuum sintering furnace, 2, stove seat, 3, footstock, 4, workbench, 5, quartz container,
6, with crystalline phase core shell structure beta-molecular sieve, 7, resistance heater, 8, outer water circulating cooling pipe,
9, water inlet, 10, delivery port, 11, pipe valve of giving vent to anger, 12, display screen, 13, indicator lamp,
14, power switch, 15, heating temperature control, 16, controller for vacuum pump, 17, heating
Time controller, 18, vavuum pump, 19, vacuum tube, 20, vacuum valve, 21, argon bottle,
22, tunger tube, 23, argon gas valve, 24, argon gas, 25, furnace chamber.
Detailed description of the invention
Below in conjunction with accompanying drawing, the present invention will be further described:
Shown in Fig. 1, for same crystalline phase core shell structure beta-molecular sieve vacuum baking state diagram, each position
Put, annexation wants correct, proportioning according to quantity, sequentially operates.
The value of chemical substance that preparation uses is to determine by the scope pre-set, with gram,
Milliliter, centimetre3For measurement unit.
Carry out in vacuum sintering furnace with the roasting of crystalline phase core shell structure beta-molecular sieve, be
Heat, vacuumize, argon shield, complete under outer water circulating cooling；
Vacuum sintering furnace 1 is vertical rectangle, is stove seat 2 in the bottom of vacuum sintering furnace 1, on
Portion is footstock 3；The external rings of vacuum sintering furnace 1 is around arranging outer water circulating cooling pipe 8, and connects
Tap into the mouth of a river 9, delivery port 10；The inside of vacuum sintering furnace 1 is furnace chamber 25, on inwall
Be provided with resistance heater 7, inner bottom part is provided with workbench 4, is provided with quartz appearance on workbench 4
Device 5, is same crystalline phase core shell structure beta-molecular sieve 6 in quartz container 5, at vacuum sintering furnace 1
Upper right quarter be provided with pipe valve 11 of giving vent to anger；Stove seat 2 is provided with display screen 12, indicator lamp 13,
Power switch 14, heating temperature control 15, controller for vacuum pump 16, heat time control
Device 17；Right lower quadrant at vacuum sintering furnace 1 is provided with vavuum pump 18, and vavuum pump 18 passes through vacuum
Pipe 19, vacuum valve 20 connect with furnace chamber 25；Left part at vacuum sintering furnace 1 is provided with argon gas
Bottle 21, argon bottle 21 is goed deep in furnace chamber 25 by argon gas valve 23, tunger tube 22, and to stove
Input argon gas 24 in chamber 25.
Shown in Fig. 2, for same crystalline phase core shell structure beta-molecular sieve shape appearance figure, as seen from the figure, Zuo Tu
Amplifying shape appearance figure for nuclear phase beta-molecular sieve monomer, compound with regular structure, surface smooth, and right figure is the isomorphous
Phase core shell structure beta-molecular sieve shape appearance figure, the basic crystal configuration keeping nuclear phase beta-molecular sieve,
One layer of fine and close shell phase nano beta molecular sieve it is wrapped on nuclear phase molecular sieve.
Shown in Fig. 3, for same crystalline phase core shell structure beta-molecular sieve X-ray diffraction intensity spectrogram,
As seen from the figure, the same crystalline phase core shell structure beta-molecular sieve of synthesis demonstrates its distinctive feature diffraction
Peak, peak type is sharp-pointed and without other miscellaneous peaks, and diffracted intensity is higher.
Claims (2)
1. the preparation method with crystalline phase core shell structure beta-molecular sieve, it is characterized in that: the chemical substance material of use is: white carbon, tetraethyl orthosilicate, sodium metaaluminate, ammonium fluoride, tetraethyl ammonium hydroxide, deionized water, argon gas, it is as follows that it prepares consumption: with gram, milliliter, centimetre3For measurement unit
White carbon: SiO2, 2g ± 0.001g
Tetraethyl orthosilicate: Si (OC2H5)4, 20.79mL ± 0.01mL
Sodium metaaluminate: NaAlO2, 0.171g ± 0.001g
Ammonium fluoride: NH4F, 1.891g ± 0.001g
Tetraethyl ammonium hydroxide: (C2H5)4NOH, concentration 25%, 80mL ± 0.01mL
Deionized water: H2O, 5000mL ± 50mL
Argon gas: Ar, 100000cm3±100cm3
Preparation method is as follows:
(1) configuration inorganic agent
Measure tetraethyl ammonium hydroxide 5.89mL ± 0.01mL, deionized water 24.11mL ± 0.01mL, add in beaker, stir 30min, become the tetraethyl ammonium hydroxide aqueous solution 30mL of 0.341mol/L；
(2) nuclear phase beta-molecular sieve is prepared
1. preparation nuclear phase beta-molecular sieve mixed solution
Measure tetraethyl orthosilicate 20.79mL ± 0.01mL, deionized water 5mL ± 0.01mL, tetraethyl ammonium hydroxide 28mL ± 0.01mL, weigh ammonium fluoride 1.891g ± 0.001g, add in beaker, it is stirred, mixing time 300min, the volatile materials making mixture produce fully volatilizees, and forms white gels mixed solution；
2. heating crystallization
The white gels mixed solution of preparation is moved in polytetrafluoroethylcontainer container, is subsequently placed in reactor, and airtight；
Reactor is placed in airtight heating in insulating box, heating-up temperature 150 DEG C ± 2 DEG C, constant temperature, insulation, static crystallization 120h, becomes crystallization gel solution；
3. quenching
After reaction terminates, close insulating box, take out reactor and be placed in quenching groove, the deionized water of 10 DEG C is quickly cooled to 20 DEG C；
4. centrifugation
Open reactor, take out polytetrafluoroethylcontainer container, the crystallization gel solution in polytetrafluoroethylcontainer container is placed in centrifuge tube, be centrifuged separating, centrifugation revolution 5000r/min, disengaging time 20min, retain solid sediment after centrifugation, discard supernatant；
5. it is vacuum dried
Solid sediment is placed in evaporating dish, is subsequently placed in vacuum drying chamber and is dried, baking temperature 120 DEG C, vacuum 10Pa, drying time 6h, dried nuclear phase beta-molecular sieve powder 6g ± 0.001g；
(3) pretreatment nuclear phase beta-molecular sieve
1. preparation pretreatment nuclear phase beta-molecular sieve solution
By nuclear phase beta-molecular sieve powder 5g ± 0.001g, tetraethyl ammonium hydroxide aqueous solution 25mL ± 0.01mL, add in polytetrafluoroethylcontainer container, be stirred vigorously 1h, obtain mixed solution；
2. isothermal reaction
The polytetrafluoroethylcontainer container filling mixed solution is put in reactor and airtight, reactor is placed in insulating box heating, heating-up temperature 100 DEG C ± 2 DEG C, constant temperature, insulation, static reaction 24h；
3. quenching
Stop heating after reaction, move to reactor, in quenching groove, the deionized water of 10 DEG C be quickly cooled to 20 DEG C；
4. wash
Open reactor, the mixed solution in polytetrafluoroethylcontainer container is poured in beaker, add deionized water 500mL, agitator treating 10min, become cleaning solution；
5. centrifugation
Cleaning solution is placed in centrifuge tube, is centrifuged separating, centrifugation revolution 5000r/min, disengaging time 20min, after centrifugation, retain solid sediment, discard supernatant；
6. it is vacuum dried
Solid sediment is placed in evaporating dish, be subsequently placed in vacuum drying chamber be dried, baking temperature 120 DEG C, vacuum 10Pa, drying time 6h, the dried nuclear phase beta-molecular sieve powder 4.5g ± 0.001g that must pre-process；
(4) preparation is with crystalline phase core shell structure beta-molecular sieve
1. same crystalline phase core shell structure beta-molecular sieve mixed solution is prepared
Measure deionized water 3.1mL ± 0.01mL, tetraethyl ammonium hydroxide 11.52mL ± 0.01mL, weigh sodium metaaluminate 0.171g ± 0.001g, white carbon 2g ± 0.001g joins in polytetrafluoroethylcontainer container, use heat collecting type constant temperature blender with magnetic force heated at constant temperature stirring 2h, heating-up temperature 80 DEG C ± 2 DEG C, agitation revolution 600r/min, make mixture fully dissolve, form clear gel solution；In gel solution, add the nuclear phase beta-molecular sieve 4g ± 0.001g of pretreatment, continue stirring 30min, become mixed solution；
2. static crystallization is heated
The polytetrafluoroethylcontainer container filling mixed solution is placed in reactor, and airtight, then reactor is put in insulating box and heat, heating-up temperature 140 DEG C ± 2 DEG C, constant temperature, static crystallization reaction 48h；
3. quenching
After crystallization, stop heating, open insulating box, take out reactor, be placed in quenching groove, the deionized water of 10 DEG C is quickly cooled to 20 DEG C；
4. deionized water dilution, centrifugation
Open reactor after cooling, the mixed solution in polytetrafluoroethylcontainer container is poured in beaker, add deionized water 500mL, magnetic stirring apparatus stirs 30min, becomes dilution mixture solution；
Dilution mixture solution is placed in the centrifuge tube of centrifuge, is centrifuged separating, centrifugation revolution 8000r/min, centrifugation time 30min, after centrifugation, retain sediment, discard supernatant；
5. dispersion, centrifugation are cleaned
Putting the precipitate in beaker, add deionized water 500mL, be subsequently placed in ultrasonic wave separating apparatus, carry out ultrasonic cleaning and dispersion, ultrasonic frequency is 40kHz, jitter time 30min；
Then dispersion soln is placed in the centrifuge tube of centrifuge and is centrifuged separating, centrifugation revolution 8000r/min, centrifugation time 30min, retain sediment, discard supernatant after centrifugation；
Clean dispersion, centrifugation repeats 3 times；
6. vacuum baking
Carry out in vacuum sintering furnace with the roasting of crystalline phase core shell structure beta-molecular sieve, heating, vacuumize, argon shield, complete under outer water circulating cooling；
Put the precipitate in quartz container, be subsequently placed on the workbench in vacuum sintering furnace；
Closing vacuum sintering furnace, open vavuum pump, extract furnace air, in making stove, pressure reaches 5Pa；
Opening argon bottle, tunger tube, be passed through argon gas in stove, in making stove, invariablenes pressure of liquid is at 0.09MPa；
Open outer water circulating cooling pipe, carry out outer water circulating cooling；
Opening resistor heater, heating-up temperature 550 DEG C ± 2 DEG C, carry out roasting, heat roasting time 300min；
Stopping heating after roasting, the product in quartz container cools to 25 DEG C with the furnace；
Must be with crystalline phase core shell structure beta-molecular sieve after cooling；
(5) detect, analyze, characterize
The crystal structure of same crystalline phase core shell structure beta-molecular sieve, the grain morphology of preparation is detected, analyzes, characterizes；
Crystalline product morphology analysis is carried out by SEM；
Crystalline product thing phase and crystallinity analysis is carried out with X-ray diffractometer；
Conclusion: be white powder with crystalline phase core shell structure beta-molecular sieve, powder granule diameter 15～20 μm, extra-granular is wrapped up by nanocrystal, and inside is micron grain, and for core shell structure, product parcel degree reaches 97%, and product purity reaches 99.9%；
(6) store
The same crystalline phase core shell structure beta-molecular sieve white powder of preparation is put in valve bag and seals, valve bag is stored in the glass container of amber transparent, seals lucifuge and store, need protection against the tide, acid-alkali salt class material sun-proof, anti-to corrode, storage temperature 20 DEG C, relative humidity≤10%.
The preparation method of a kind of same crystalline phase core shell structure beta-molecular sieve the most according to claim 1; it is characterized in that: carry out in vacuum sintering furnace with the roasting of crystalline phase core shell structure beta-molecular sieve, heating, vacuumize, argon shield, complete under outer water circulating cooling；
Vacuum sintering furnace (1) is vertical rectangle, is stove seat (2) in the bottom of vacuum sintering furnace (1), and top is footstock (3)；The external rings of vacuum sintering furnace (10) is around arranging outer water circulating cooling pipe (8), and connects water inlet (9), delivery port (10)；The inside of vacuum sintering furnace (1) is furnace chamber (25), be provided with resistance heater (7) on inwall, inner bottom part is provided with workbench (4), workbench (4) is provided with quartz container (5), being same crystalline phase core shell structure beta-molecular sieve (6) in quartz container (5), the upper right quarter at vacuum sintering furnace (1) is provided with pipe valve of giving vent to anger (11)；Stove seat (2) is provided with display screen (12), indicator lamp (13), power switch (14), heating temperature control (15), controller for vacuum pump (16), heat time controller (17)；Right lower quadrant at vacuum sintering furnace (1) is provided with vavuum pump (18), and vavuum pump (18) is connected with furnace chamber (25) by vacuum tube (19), vacuum valve (20)；Left part at vacuum sintering furnace (1) is provided with argon bottle (21), argon bottle (21) is goed deep in furnace chamber (25) by argon gas valve (23), tunger tube (22), and inputs argon gas (24) in furnace chamber (25).
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| CN101177276B (en) * | 2007-11-03 | 2010-06-16 | 太原理工大学 | Core-shell structural dibasic composite zeolite and preparation method thereof |
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