CN104760972A - Preparation method of isomorphous-phase core-shell structured beta-molecular sieve - Google Patents
Preparation method of isomorphous-phase core-shell structured beta-molecular sieve Download PDFInfo
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Abstract
The invention relates to a preparation method of an isomorphous-phase core-shell structured beta-molecular sieve, which is implemented by taking white carbon black, tetraethylortho silicate, sodium metaaluminate, tetraethylammonium hydroxide, and ammonium fluoride as raw materials and taking a tetraethylammonium hydroxide aqueous solution as a treating agent through the steps of synthesizing a nuclear-phase beta-molecular sieve firstly; carrying out mixed liquid preparation, and crystallizing the obtained object in a reaction kettle; and sequentially carrying out constant-temperature heating, quenching, cleaning and dispersing, centrifugal separation, vacuum drying, and high-temperature vacuum calcination on the obtained product, so that the isomorphous-phase core-shell structured beta-molecular sieve is obtained. The preparation method is advanced in process and detailed and accurate in data, the crystal diameter of the prepared isomorphous-phase core-shell structured molecular sieve is 15-20 mu m, the outside of each crystal is tightly wrapped with a nanocrystal, the wrapping degree of product reaches 97%, and the product purity reaches 99.9%, so that the molecular sieve can be matched with various chemical substances and then the obtained objects are used as catalysts, therefore, the method disclosed by the invention is an extremely ideal preparation method of an isomorphous-phase core-shell structured beta-molecular sieve.
Description
Technical field
The present invention relates to a kind of preparation method of same crystalline phase nucleocapsid structure beta-molecular sieve, belong to the technical field of zeolite compound catalyze material preparations and applicatio.
Background technology
Beta-molecular sieve has unique topological framework, it is a kind of high-silica zeolite with three-dimensional twelve-ring pore passage structure, there is good thermostability, hydrophobicity, acid resistance, anti-coking, be widely used in hydrocracking, hydrocarbon isomerization, alkylating aromatic hydrocarbon, purifying vehicle exhaust catalytic process.
In catalytic process, beta-molecular sieve area carbon is the major cause causing its catalyst deactivation, at present, along with the further investigation to nanotechnology, nano beta molecular sieve is because of its larger specific surface area, shorter pore passage structure and more surfactivity, make it weaken and even eliminate carbon distribution problem, but also there is many shortcomings in the process preparing nano beta molecular sieve, oxidizable moisture absorption, easily reunion, poor stability; Micron order large grain size beta-molecular sieve can provide longer the evolving path, can play regulating effect to catalyzed reaction; There is many drawbacks in the beta-molecular sieve of existing single structure, constrains application industrially.
Summary of the invention
Goal of the invention
The object of the invention is the situation for background technology and deficiency, with white carbon black, tetraethoxy, sodium metaaluminate for raw material, first prepare nuclear phase beta-molecular sieve, through static crystallization, quenching, separation, vacuum baking, make the same crystalline phase nucleocapsid structure beta-molecular sieve of band coating layer, to increase substantially the purity of nucleocapsid structure beta-molecular sieve, to expand the range of application of beta-molecular sieve.
Technical scheme
The chemical substance material that the present invention uses is: white carbon black, tetraethoxy, sodium metaaluminate, Neutral ammonium fluoride, tetraethyl ammonium hydroxide, deionized water, argon gas, and it is as follows that it prepares consumption: with gram, milliliter, centimetre
3for measure unit
White carbon black: SiO
2, 2g ± 0.001g
Tetraethoxy: Si (OC
2h
5)
4, 20.79mL ± 0.01mL
Sodium metaaluminate: NaAlO
2, 0.171g ± 0.001g
Neutral ammonium fluoride: NH
4f, 1.891g ± 0.001g
Tetraethyl ammonium hydroxide: (C
2h
5)
4nOH, concentration 25%, 80mL ± 0.01mL
Deionized water: H
2o, 5000mL ± 50mL
Argon gas: Ar, 100000cm
3± 100cm
3
Preparation method is as follows:
(1) configuration process 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. nuclear phase beta-molecular sieve mixing solutions is prepared
Measure tetraethoxy 20.79mL ± 0.01mL, deionized water 5mL ± 0.01mL, tetraethyl ammonium hydroxide 28mL ± 0.01mL, take Neutral ammonium fluoride 1.891g ± 0.001g, add in beaker, stir, churning time 300min, the volatile matter that mixture is produced fully volatilizees, and forms white gels mixing solutions;
2. heating crystallization
The white gels mixing solutions of preparation is moved in polytetrafluoroethylcontainer container, is then placed in reactor, and airtight;
Reactor is placed in the airtight heating of thermostat container, Heating temperature 150 DEG C ± 2 DEG C, constant temperature, insulation, static crystallization 120h, becomes crystallization gelating soln;
3. quenching
After reaction terminates, close thermostat container, take out reactor and be placed in quenching groove, in the deionized water of 10 DEG C, be quickly cooled to 20 DEG C;
4. centrifugation
Open reactor, take out polytetrafluoroethylcontainer container, the crystallization gelating soln in polytetrafluoroethylcontainer container is placed in centrifuge tube, carry out centrifugation, centrifugation revolution 5000r/min, disengaging time 20min, retain solid sediment after centrifugation, discard supernatant liquor;
5. vacuum-drying
Solid sediment is placed in furnace pot, is then placed in vacuum drying oven dry, drying temperature 120 DEG C, vacuum tightness 10Pa, time of drying, 6h, obtained nuclear phase beta-molecular sieve powder 6g ± 0.001g after drying;
(3) pre-treatment nuclear phase beta-molecular sieve
1. pre-treatment nuclear phase beta-molecular sieve solution is prepared
By nuclear phase beta-molecular sieve powder 5g ± 0.001g, tetraethyl ammonium hydroxide aqueous solution 25mL ± 0.01mL, adds in polytetrafluoroethylcontainer container, vigorous stirring 1h, obtains mixing solutions;
2. isothermal reaction
The polytetrafluoroethylcontainer container filling mixing solutions is put into reactor and airtight, reactor is placed in thermostat container and heats, Heating temperature 100 DEG C ± 2 DEG C, constant temperature, insulation, static reaction 24h;
3. quenching
Stop heating after reaction, reactor is moved in quenching groove, in the deionized water of 10 DEG C, be quickly cooled to 20 DEG C;
4. wash
Open reactor, the mixing solutions in polytetrafluoroethylcontainer container is poured in beaker, adds deionized water 500mL, agitator treating 10min, become washings;
5. centrifugation
Washings is placed in centrifuge tube, carries out centrifugation, centrifugation revolution 5000r/min, disengaging time 20min, after centrifugation, retain solid sediment, discard supernatant liquor;
6. vacuum-drying
Solid sediment is placed in furnace pot, is then placed in vacuum drying oven dry, drying temperature 120 DEG C, vacuum tightness 10Pa, time of drying, 6h, obtained pretreated nuclear phase beta-molecular sieve powder 4.5g ± 0.001g after drying;
(4) preparation is with crystalline phase nucleocapsid structure beta-molecular sieve
1. same crystalline phase nucleocapsid structure beta-molecular sieve mixing solutions is prepared
Measure deionized water 3.1mL ± 0.01mL, tetraethyl ammonium hydroxide 11.52mL ± 0.01mL, take sodium metaaluminate 0.171g ± 0.001g, white carbon black 2g ± 0.001g joins in polytetrafluoroethylcontainer container, heat collecting type constant temperature blender with magnetic force thermostatically heating is adopted to stir 2h, Heating temperature 80 DEG C ± 2 DEG C, agitation revolution 600r/min, mixture is fully dissolved, forms clear gel solution; In gelating soln, add pretreated nuclear phase molecular sieve 4g ± 0.001g, continue to stir 30min, become mixing solutions;
2. static crystallization is heated
The polytetrafluoroethylcontainer container filling mixing solutions is placed in reactor, and airtight, then reactor is put into thermostat container and heat, Heating temperature 140 DEG C ± 2 DEG C, constant temperature, static crystallization reaction 48h;
3. quenching
After crystallization, stop heating, open thermostat container, take out reactor, be placed in quenching groove, in the deionized water of 10 DEG C, be quickly cooled to 20 DEG C;
4. deionized water dilution, centrifugation
Open reactor after cooling, the mixing solutions in polytetrafluoroethylcontainer container is poured in beaker, add deionized water 500mL, magnetic stirring apparatus stirs 30min, become dilution mixture solution;
Dilution mixture solution is placed in the centrifuge tube of whizzer, carries out centrifugation, centrifugation revolution 8000r/min, centrifugation time 30min, after centrifugation, retain throw out, discard supernatant liquor;
5. dispersion, centrifugation is cleaned
Throw out is placed in beaker, adds deionized water 500mL, be then placed in ultrasonic wave separating apparatus, carry out ultrasonic cleaning and dispersion, ultrasonic frequency is 40KHz, jitter time 30min;
Then centrifuge tube dispersion soln being placed in whizzer carries out centrifugation, centrifugation revolution 8000r/min, and centrifugation time 30min, retains throw out after centrifugation, discard supernatant liquor;
Cleaning dispersion, centrifugation repeat 3 times;
6. vacuum baking
Roasting with crystalline phase nucleocapsid structure beta-molecular sieve is carried out in vacuum sintering furnace, heating, vacuumizes, argon shield, to complete under the cooling of outer water cycle;
Throw out is placed in quartz container, is then placed on the worktable in vacuum sintering furnace;
Close vacuum sintering furnace, open vacuum pump, extract furnace air, make pressure in stove reach 5Pa;
Open argon bottle, tunger tube, in stove, pass into argon gas, to make in stove invariablenes pressure of liquid at 0.09MPa;
Open outer water cycle cooling tube, carry out outer water cycle cooling;
Opening resistor well heater, Heating temperature 550 DEG C ± 2 DEG C, carries out roasting, heating roasting time 300min;
Cooling, stop heating after roasting, the product in quartz container, cools to 25 DEG C with the furnace;
Must with crystalline phase nucleocapsid structure beta-molecular sieve after cooling;
(5) detect, analyze, characterize
The crystalline structure of same crystalline phase nucleocapsid structure beta-molecular sieve of preparation, grain morphology are detected, analyze, characterized;
Crystalline product morphology analysis is carried out by scanning electronic microscope;
Crystalline product thing phase and crystallinity analysis is carried out with X-ray diffractometer;
Conclusion: be white powder with crystalline phase nucleocapsid structure beta-molecular sieve, powder granule diameter 15 ~ 20 μm, extra-granular is wrapped up by nanocrystal, and inside is micron grain, is nucleocapsid structure, and product parcel degree reaches 97%, and product purity reaches 99.9%;
(6) store
The same crystalline phase nucleocapsid structure beta-molecular sieve white powder of preparation is put into valve bag seal, be stored in by valve bag in the Glass Containers of amber transparent, sealing lucifuge stores, and needs protection against the tide, sun-proof, anti-acid-alkali salt class matter corrodes, storing temp 20 DEG C, relative humidity≤10%.
Beneficial effect
The present invention has obvious advance compared with background technology, with white carbon black, tetraethoxy, sodium metaaluminate, tetraethyl ammonium hydroxide, Neutral ammonium fluoride is raw material, with the tetraethyl ammonium hydroxide aqueous solution for treatment agent, take deionized water as solvent, washing composition, first synthesize nuclear phase beta-molecular sieve, then with treatment agent, nuclear phase beta-molecular sieve is processed, finally synthesize same crystalline phase nucleocapsid structure beta-molecular sieve, through Compound mixed solution, reactor crystallization, thermostatically heating, quenching, cleaning dispersion, centrifugation, vacuum-drying, high-temperature vacuum roasting, make same crystalline phase nucleocapsid structure beta-molecular sieve, this preparation method's technique is advanced, data are accurately full and accurate, the same crystalline phase nucleocapsid structure zeolite crystal diameter 15 ~ 20 μm of preparation, the outside nanocrystal parcel of crystal grain closely, product parcel degree reaches 97%, product purity reaches 99.9%, can mate with number of chemical material and make catalyzer and use, it is the very good preparation method with crystalline phase nucleocapsid structure beta-molecular sieve.
Accompanying drawing explanation
Fig. 1 is the state graph of same crystalline phase nucleocapsid structure beta-molecular sieve vacuum baking
Fig. 2 is same crystalline phase nucleocapsid structure beta-molecular sieve shape appearance figure
Fig. 3 is same crystalline phase nucleocapsid 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, worktable, 5, quartz container, 6, with crystalline phase nucleocapsid structure beta-molecular sieve, 7, resistance heater, 8, outer water cycle cooling tube, 9, water-in, 10, water outlet, 11, pipe valve of giving vent to anger, 12, display screen, 13, pilot lamp, 14, power switch, 15, heating temperature control, 16, controller for vacuum pump, 17, heat-up time controller, 18, vacuum pump, 19, valve tube, 20, vacuum valve, 21, argon bottle, 22, tunger tube, 23, argon gas valve, 24, argon gas, 25, furnace chamber.
Embodiment
Below in conjunction with accompanying drawing, the present invention will be further described:
Shown in Fig. 1, be the state graph of same crystalline phase nucleocapsid structure beta-molecular sieve vacuum baking, each position, annexation want correct, and proportioning according to quantity, operates according to the order of sequence.
The value of the chemical substance that preparation uses determines by the scope pre-set, with gram, milliliter, centimetre
3for measure unit.
Roasting with crystalline phase nucleocapsid structure beta-molecular sieve is carried out in vacuum sintering furnace, heating, vacuumizes, argon shield, to complete under the cooling of outer water cycle;
Vacuum sintering furnace 1 is vertical rectangle, and be stove seat 2 in the bottom of vacuum sintering furnace 1, top is footstock 3; Outer water cycle cooling tube 8 is put in the external rings winding of vacuum sintering furnace 1, and connects water-in 9, water outlet 10; The inside of vacuum sintering furnace 1 is furnace chamber 25, inwall is provided with resistance heater 7, inner bottom part is provided with worktable 4, worktable 4 is provided with quartz container 5, is same crystalline phase nucleocapsid structure beta-molecular sieve 6 in quartz container 5, is provided with at the upper right quarter of vacuum sintering furnace 1 pipe valve 11 of giving vent to anger; Stove seat 2 is provided with display screen 12, pilot lamp 13, power switch 14, heating temperature control 15, controller for vacuum pump 16, heat-up time controller 17; Be provided with vacuum pump 18 at the right lower quadrant of vacuum sintering furnace 1, vacuum pump 18 is communicated with furnace chamber 25 by valve tube 19, vacuum valve 20; Be provided with argon bottle 21 at the left part of vacuum sintering furnace 1, 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.
Shown in Fig. 2, for same crystalline phase nucleocapsid structure beta-molecular sieve shape appearance figure, as seen from the figure, left figure is that nuclear phase beta-molecular sieve monomer amplifies shape appearance figure, compound with regular structure, surface smoothing, right figure is same crystalline phase nucleocapsid structure beta-molecular sieve shape appearance figure, and the basic crystal configuration keeping nuclear phase beta-molecular sieve, nuclear phase molecular sieve is wrapped in the shell phase nano beta molecular sieve of one deck densification.
Shown in Fig. 3, be same crystalline phase nucleocapsid structure beta-molecular sieve X-ray diffraction intensity spectrogram, as seen from the figure, the same crystalline phase nucleocapsid structure beta-molecular sieve of synthesis demonstrates its distinctive characteristic diffraction peak, and peak type is sharp-pointed and without other assorted peaks, diffracted intensity is higher.
Claims (2)
1. the preparation method with crystalline phase nucleocapsid structure beta-molecular sieve, it is characterized in that: the chemical substance material of use is: white carbon black, tetraethoxy, sodium metaaluminate, Neutral ammonium fluoride, tetraethyl ammonium hydroxide, deionized water, argon gas, it is as follows that it prepares consumption: with gram, milliliter, centimetre
3for measure unit
White carbon black: SiO
2, 2g ± 0.001g
Tetraethoxy: Si (OC
2h
5)
4, 20.79mL ± 0.01mL
Sodium metaaluminate: NaAlO
2, 0.171g ± 0.001g
Neutral ammonium fluoride: NH
4f, 1.891g ± 0.001g
Tetraethyl ammonium hydroxide: (C
2h
5)
4nOH, concentration 25%, 80mL ± 0.01mL
Deionized water: H
2o, 5000mL ± 50mL
Argon gas: Ar, 100000cm
3± 100cm
3
Preparation method is as follows:
(1) configuration process 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. nuclear phase beta-molecular sieve mixing solutions is prepared
Measure tetraethoxy 20.79mL ± 0.01mL, deionized water 5mL ± 0.01mL, tetraethyl ammonium hydroxide 28mL ± 0.01mL, take Neutral ammonium fluoride 1.891g ± 0.001g, add in beaker, stir, churning time 300min, the volatile matter that mixture is produced fully volatilizees, and forms white gels mixing solutions;
2. heating crystallization
The white gels mixing solutions of preparation is moved in polytetrafluoroethylcontainer container, is then placed in reactor, and airtight;
Reactor is placed in the airtight heating of thermostat container, Heating temperature 150 DEG C ± 2 DEG C, constant temperature, insulation, static crystallization 120h, becomes crystallization gelating soln;
3. quenching
After reaction terminates, close thermostat container, take out reactor and be placed in quenching groove, in the deionized water of 10 DEG C, be quickly cooled to 20 DEG C;
4. centrifugation
Open reactor, take out polytetrafluoroethylcontainer container, the crystallization gelating soln in polytetrafluoroethylcontainer container is placed in centrifuge tube, carry out centrifugation, centrifugation revolution 5000r/min, disengaging time 20min, retain solid sediment after centrifugation, discard supernatant liquor;
5. vacuum-drying
Solid sediment is placed in furnace pot, is then placed in vacuum drying oven dry, drying temperature 120 DEG C, vacuum tightness 10Pa, time of drying, 6h, obtained nuclear phase beta-molecular sieve powder 6g ± 0.001g after drying;
(3) pre-treatment nuclear phase beta-molecular sieve
1. pre-treatment nuclear phase beta-molecular sieve solution is prepared
By nuclear phase beta-molecular sieve powder 5g ± 0.001g, tetraethyl ammonium hydroxide aqueous solution 25mL ± 0.01mL, adds in polytetrafluoroethylcontainer container, vigorous stirring 1h, obtains mixing solutions;
2. isothermal reaction
The polytetrafluoroethylcontainer container filling mixing solutions is put into reactor and airtight, reactor is placed in thermostat container and heats, Heating temperature 100 DEG C ± 2 DEG C, constant temperature, insulation, static reaction 24h;
3. quenching
Stop heating after reaction, reactor is moved in quenching groove, in the deionized water of 10 DEG C, be quickly cooled to 20 DEG C;
4. wash
Open reactor, the mixing solutions in polytetrafluoroethylcontainer container is poured in beaker, adds deionized water 500mL, agitator treating 10min, become washings;
5. centrifugation
Washings is placed in centrifuge tube, carries out centrifugation, centrifugation revolution 5000r/min, disengaging time 20min, after centrifugation, retain solid sediment, discard supernatant liquor;
6. vacuum-drying
Solid sediment is placed in furnace pot, is then placed in vacuum drying oven dry, drying temperature 120 DEG C, vacuum tightness 10Pa, time of drying, 6h, obtained pretreated nuclear phase beta-molecular sieve powder 4.5g ± 0.001g after drying;
(4) preparation is with crystalline phase nucleocapsid structure beta-molecular sieve
1. same crystalline phase nucleocapsid structure beta-molecular sieve mixing solutions is prepared
Measure deionized water 3.1mL ± 0.01mL, tetraethyl ammonium hydroxide 11.52mL ± 0.01mL, take sodium metaaluminate 0.171g ± 0.001g, white carbon black 2g ± 0.001g joins in polytetrafluoroethylcontainer container, heat collecting type constant temperature blender with magnetic force thermostatically heating is adopted to stir 2h, Heating temperature 80 DEG C ± 2 DEG C, agitation revolution 600r/min, mixture is fully dissolved, forms clear gel solution; In gelating soln, add pretreated nuclear phase molecular sieve 4g ± 0.001g, continue to stir 30min, become mixing solutions;
2. static crystallization is heated
The polytetrafluoroethylcontainer container filling mixing solutions is placed in reactor, and airtight, then reactor is put into thermostat container and heat, Heating temperature 140 DEG C ± 2 DEG C, constant temperature, static crystallization reaction 48h;
3. quenching
After crystallization, stop heating, open thermostat container, take out reactor, be placed in quenching groove, in the deionized water of 10 DEG C, be quickly cooled to 20 DEG C;
4. deionized water dilution, centrifugation
Open reactor after cooling, the mixing solutions in polytetrafluoroethylcontainer container is poured in beaker, add deionized water 500mL, magnetic stirring apparatus stirs 30min, become dilution mixture solution;
Dilution mixture solution is placed in the centrifuge tube of whizzer, carries out centrifugation, centrifugation revolution 8000r/min, centrifugation time 30min, after centrifugation, retain throw out, discard supernatant liquor;
5. dispersion, centrifugation is cleaned
Throw out is placed in beaker, adds deionized water 500mL, be then placed in ultrasonic wave separating apparatus, carry out ultrasonic cleaning and dispersion, ultrasonic frequency is 40KHz, jitter time 30min;
Then centrifuge tube dispersion soln being placed in whizzer carries out centrifugation, centrifugation revolution 8000r/min, and centrifugation time 30min, retains throw out after centrifugation, discard supernatant liquor;
Cleaning dispersion, centrifugation repeat 3 times;
6. vacuum baking
Roasting with crystalline phase nucleocapsid structure beta-molecular sieve is carried out in vacuum sintering furnace, heating, vacuumizes, argon shield, to complete under the cooling of outer water cycle;
Throw out is placed in quartz container, is then placed on the worktable in vacuum sintering furnace;
Close vacuum sintering furnace, open vacuum pump, extract furnace air, make pressure in stove reach 5Pa;
Open argon bottle, tunger tube, in stove, pass into argon gas, to make in stove invariablenes pressure of liquid at 0.09MPa;
Open outer water cycle cooling tube, carry out outer water cycle cooling;
Opening resistor well heater, Heating temperature 550 DEG C ± 2 DEG C, carries out roasting, heating roasting time 300min;
Cooling, stop heating after roasting, the product in quartz container, cools to 25 DEG C with the furnace;
Must with crystalline phase nucleocapsid structure beta-molecular sieve after cooling;
(5) detect, analyze, characterize
The crystalline structure of same crystalline phase nucleocapsid structure beta-molecular sieve of preparation, grain morphology are detected, analyze, characterized;
Crystalline product morphology analysis is carried out by scanning electronic microscope;
Crystalline product thing phase and crystallinity analysis is carried out with X-ray diffractometer;
Conclusion: be white powder with crystalline phase nucleocapsid structure beta-molecular sieve, powder granule diameter 15 ~ 20 μm, extra-granular is wrapped up by nanocrystal, and inside is micron grain, is nucleocapsid structure, and product parcel degree reaches 97%, and product purity reaches 99.9%;
(6) store
The same crystalline phase nucleocapsid structure beta-molecular sieve white powder of preparation is put into valve bag seal, be stored in by valve bag in the Glass Containers of amber transparent, sealing lucifuge stores, and needs protection against the tide, sun-proof, anti-acid-alkali salt class matter corrodes, storing temp 20 DEG C, relative humidity≤10%.
2. the preparation method of a kind of same crystalline phase nucleocapsid structure beta-molecular sieve according to claim 1, it is characterized in that: the roasting with crystalline phase nucleocapsid structure beta-molecular sieve is carried out in vacuum sintering furnace, heating, vacuumize, argon shield, to complete under the cooling of outer water cycle;
Vacuum sintering furnace (1) is vertical rectangle, and be stove seat (2) in the bottom of vacuum sintering furnace (1), top is footstock (3); Outer water cycle cooling tube (8) is put in the external rings winding of vacuum sintering furnace (10), and connects water-in (9), water outlet (10); The inside of vacuum sintering furnace (1) is furnace chamber (25), inwall is provided with resistance heater (7), inner bottom part is provided with worktable (4), worktable (4) is provided with quartz container (5), be same crystalline phase nucleocapsid structure beta-molecular sieve (6) in quartz container (5), be provided with pipe valve of giving vent to anger (11) at the upper right quarter of vacuum sintering furnace (1); Stove seat (2) is provided with display screen (12), pilot lamp (13), power switch (14), heating temperature control (15), controller for vacuum pump (16), controller heat-up time (17); Be provided with vacuum pump (18) at the right lower quadrant of vacuum sintering furnace (1), vacuum pump (18) is communicated with furnace chamber (25) by valve tube (19), vacuum valve (20); Argon bottle (21) is provided with at the left part of vacuum sintering furnace (1), argon bottle (21) is goed deep in furnace chamber (25) by argon gas valve (23), tunger tube (22), and input argon gas (24) in furnace chamber (25).
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105869922A (en) * | 2016-04-11 | 2016-08-17 | 太原理工大学 | Rapid preparation method of manganese oxide/carbon sphere composite material for three-dimensional (3D) printing |
| CN108267346A (en) * | 2016-12-30 | 2018-07-10 | 亚申科技研发中心（上海）有限公司 | The high-throughput preparation system and method for sieve sample |
| CN109772432A (en) * | 2019-02-01 | 2019-05-21 | 郑州大学 | A kind of benzene selective hydrogenation alkylation prepares cyclohexyl benzene metallic cover type catalyst and preparation method thereof, application method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1393400A (en) * | 2001-06-29 | 2003-01-29 | 中国石油天然气股份有限公司 | Process for synthesizing core-shell molecular sieve |
| CN101177276A (en) * | 2007-11-03 | 2008-05-14 | 太原理工大学 | Core-shell structural dibasic composite zeolite and preparation method thereof |
| CN101890363A (en) * | 2010-07-16 | 2010-11-24 | 复旦大学 | Preparation method for mesopore-micropore core-shell composite molecular sieve catalyst |
-
2015
- 2015-04-01 CN CN201510151336.2A patent/CN104760972B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1393400A (en) * | 2001-06-29 | 2003-01-29 | 中国石油天然气股份有限公司 | Process for synthesizing core-shell molecular sieve |
| CN101177276A (en) * | 2007-11-03 | 2008-05-14 | 太原理工大学 | Core-shell structural dibasic composite zeolite and preparation method thereof |
| CN101890363A (en) * | 2010-07-16 | 2010-11-24 | 复旦大学 | Preparation method for mesopore-micropore core-shell composite molecular sieve catalyst |
Non-Patent Citations (2)
| Title |
|---|
| QIANGQIANG ZHAO ET AL.: "Core–shell structured zeolite–zeolite composites comprising Y zeolite cores and nano-b zeolite shells: Synthesis and application in hydrocracking of VGO oil", 《CHEMICAL ENGINEERING JOURNAL》 * |
| 祁晓岚等: "核壳分子筛新材料的合成、表征及应用进展", 《石油化工》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105869922A (en) * | 2016-04-11 | 2016-08-17 | 太原理工大学 | Rapid preparation method of manganese oxide/carbon sphere composite material for three-dimensional (3D) printing |
| CN108267346A (en) * | 2016-12-30 | 2018-07-10 | 亚申科技研发中心（上海）有限公司 | The high-throughput preparation system and method for sieve sample |
| CN109772432A (en) * | 2019-02-01 | 2019-05-21 | 郑州大学 | A kind of benzene selective hydrogenation alkylation prepares cyclohexyl benzene metallic cover type catalyst and preparation method thereof, application method |
| CN109772432B (en) * | 2019-02-01 | 2022-03-11 | 郑州大学 | Metal-coated catalyst for preparing cyclohexylbenzene by benzene selective hydrogenation alkylation and preparation method and use method thereof |
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