CN106517355B - A kind of method of ultrasonic wave preparation magnetism 4A molecular sieve - Google Patents
A kind of method of ultrasonic wave preparation magnetism 4A molecular sieve Download PDFInfo
- Publication number
- CN106517355B CN106517355B CN201610993852.4A CN201610993852A CN106517355B CN 106517355 B CN106517355 B CN 106517355B CN 201610993852 A CN201610993852 A CN 201610993852A CN 106517355 B CN106517355 B CN 106517355B
- Authority
- CN
- China
- Prior art keywords
- solution
- added
- molecular sieve
- magnetic
- distilled water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 239000002808 molecular sieve Substances 0.000 title claims abstract description 83
- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 230000005389 magnetism Effects 0.000 title abstract description 54
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 131
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 85
- 238000003756 stirring Methods 0.000 claims abstract description 41
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 37
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 37
- 239000000203 mixture Substances 0.000 claims abstract description 31
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 29
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910001388 sodium aluminate Inorganic materials 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract 2
- 238000005406 washing Methods 0.000 claims abstract 2
- 239000012153 distilled water Substances 0.000 claims description 66
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 21
- 229910052708 sodium Inorganic materials 0.000 claims description 21
- 239000011734 sodium Substances 0.000 claims description 21
- 239000007788 liquid Substances 0.000 claims description 19
- 238000002425 crystallisation Methods 0.000 claims description 18
- 230000008025 crystallization Effects 0.000 claims description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 6
- 238000001179 sorption measurement Methods 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims 3
- 238000001914 filtration Methods 0.000 claims 1
- 235000019795 sodium metasilicate Nutrition 0.000 abstract description 32
- 238000010521 absorption reaction Methods 0.000 abstract description 27
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 abstract description 17
- 229910021577 Iron(II) chloride Inorganic materials 0.000 abstract description 13
- 229910021578 Iron(III) chloride Inorganic materials 0.000 abstract description 13
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 abstract description 13
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 abstract description 13
- 239000002245 particle Substances 0.000 abstract description 9
- 238000006243 chemical reaction Methods 0.000 abstract description 8
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 238000004134 energy conservation Methods 0.000 abstract description 3
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 230000000877 morphologic effect Effects 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 abstract description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract 2
- 229910052710 silicon Inorganic materials 0.000 abstract 2
- 239000010703 silicon Substances 0.000 abstract 2
- 239000003513 alkali Substances 0.000 abstract 1
- 239000002904 solvent Substances 0.000 abstract 1
- 230000010355 oscillation Effects 0.000 description 28
- 238000002156 mixing Methods 0.000 description 24
- 239000000463 material Substances 0.000 description 18
- 238000009835 boiling Methods 0.000 description 15
- 239000011343 solid material Substances 0.000 description 15
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 10
- 238000004458 analytical method Methods 0.000 description 8
- 238000002329 infrared spectrum Methods 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 238000005452 bending Methods 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 238000001228 spectrum Methods 0.000 description 5
- 239000002352 surface water Substances 0.000 description 5
- CQBLUJRVOKGWCF-UHFFFAOYSA-N [O].[AlH3] Chemical compound [O].[AlH3] CQBLUJRVOKGWCF-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 229910021536 Zeolite Inorganic materials 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000010457 zeolite Substances 0.000 description 2
- 239000002156 adsorbate Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000008396 flotation agent Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- RVPVRDXYQKGNMQ-UHFFFAOYSA-N lead(2+) Chemical compound [Pb+2] RVPVRDXYQKGNMQ-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide [Fe3O4]
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
- C01B39/14—Type A
- C01B39/16—Type A from aqueous solutions of an alkali metal aluminate and an alkali metal silicate excluding any other source of alumina or silica but seeds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
- Hard Magnetic Materials (AREA)
Abstract
The present invention provides a kind of methods of ultrasonic wave preparation magnetism 4A molecular sieve, comprising the following steps: one, by FeCl2·4H2O and FeCl3·6H2O is added to the water, and NH is added after stirring heating3·H2O obtains solidliquid mixture, then carries out magnetic absorption, washing and drying process, obtains magnetic Fe3O4；Two, directed agents are prepared；Three, it using sodium aluminate as silicon source, using sodium metasilicate as silicon source, takes water as a solvent, using sodium hydroxide as alkali source, magnetic Fe is added3O4, prepare magnetism 4A molecular sieve.The present invention prepares magnetic molecule sieve using ultrasonic Wave heating, by the way that directed agents are added, which has many advantages, such as that specific surface area height, absorption property are strong, is easy by externally-applied magnetic field, reaction solution separation.Ultrasonic wave is used to prepare magnetic molecule sieve by the present invention, can be improved chemical reaction velocity, energy conservation and environmental protection, meanwhile, directed agents are added during the preparation process, make the molecular sieve uniform particle sizes of preparation, morphological rules.
Description
Technical field
The invention belongs to technical field of molecular sieve preparation, and in particular to a kind of side of ultrasonic wave preparation magnetism 4A molecular sieve
Method.
Background technique
4A molecular sieve is because of its excellent performance, such as specific surface area height in recent years, and adsorption separation performance is strong, and catalytic is excellent
Feature has a wide range of applications basis in the industry.Domestic and foreign scholars never stopped the research of new type molecular sieve, with
Material and region of chemistry be constantly progressive the synthesis for promoting the molecular sieve of different elements compositions and different basic structural units, need
New method is studied to prepare novel molecular sieve.Magnetic is prepared by molecular sieve and magnetic ferroferric oxide are compound using ultrasonic method
Property molecular sieve have wide Research Prospects.
Molecular sieve is applied to one of inorganic porous material most in industrial production, because it is with ion exchange, selection
Property absorption, catalysis and many excellent performances such as stability is good, and be widely used in environmental protection, daily-use chemical industry, petroleum are urged
The fields such as change, application especially in the treatment of waste water increasingly highlight.But directly have using chemical raw material synthesis of molecular sieve
The deficiency of three aspects.First, at high cost；Second, the effect system of being not easy to easily separates；Third, the reaction time is long, energy consumption
It is high.The molecular sieve directly synthesized is powdered, and during molding, needs add-on type agent, and preparation cost is high and to it
Performance has an impact, in order to solve the problems, such as that fine powder shape product is separated with handled liquid difficulty in the application, in addition to using molding
Outside zeolite, floatation can also isolate the fine zeolite of load adsorbate from solution, however must add flotation agent in the process,
It will cause secondary pollution.And system with molecular sieve for preparing is long for the reaction time, and energy consumption is high.
Summary of the invention
Technical problem to be solved by the present invention lies in view of the above shortcomings of the prior art, provide a kind of ultrasonic wave preparation
The method of magnetic 4A molecular sieve.This method prepares magnetic molecule sieve using ultrasonic Wave heating, by the way that directed agents are added.The magnetic of preparation
Property molecular sieve have specific surface area high, absorption property is strong, passes through externally-applied magnetic field and is easy the advantages that separating with reaction solution.The present invention will
Ultrasonic wave is used to prepare magnetic molecule sieve, can be improved chemical reaction velocity, energy conservation and environmental protection, meanwhile, it is added during the preparation process
Directed agents make the molecular sieve uniform particle sizes of preparation, morphological rules.
In order to solve the above technical problems, the technical solution adopted by the present invention is that: a kind of ultrasonic wave preparation magnetism 4A molecular sieve
Method, which is characterized in that method includes the following steps:
Step 1: by FeCl2·4H2O and FeCl3·6H2O is added in distilled water, under the conditions of nitrogen protection with
The stirring rate of 500r/min~1000r/min is stirred, and stirring while is warming up to 75 DEG C~85 DEG C, is added after constant temperature
NH3·H2O continues to obtain solidliquid mixture after stirring 20min~40min, after the solidliquid mixture natural cooling, utilize
Magnet adsorbs the magnetisable material in solidliquid mixture, and the magnetisable material then obtained to absorption is washed repeatedly,
Temperature after dry 5h~6h, obtains magnetic Fe under conditions of being 65 DEG C~75 DEG C3O4；
Step 2: sodium metasilicate is dissolved in distilled water, solution A is obtained after mixing evenly, sodium aluminate and sodium hydroxide is molten
In distilled water, solution B is obtained after mixing evenly, then solution B is added in solution A and stirs 30min, is aged 18h later,
Obtain directed agents；The mass ratio of the solution A and solution B is (1.10~1.35): 1；
Step 3: sodium metaaluminate and sodium hydroxide are dissolved in distilled water, after mixing through supersonic oscillations, obtain molten
Liquid C, sodium metasilicate and sodium hydroxide are dissolved in distilled water, after mixing through supersonic oscillations, obtain solution D, then super
Under conditions of sonication, solution D is added drop-wise in solution C with the drop rate of 2.5mL/min, continues ultrasound after being added dropwise
Wave vibrates 40min~60min, obtains gel；The concentration of sodium metaaluminate is 96g/L~100g/L, sodium hydroxide in the solution C
Concentration be 20g/L~28g/L, the concentration of sodium metasilicate is 72g/L~76g/L in the solution D, and the concentration of sodium hydroxide is
20g/L~28g/L；The mass ratio of sodium metasilicate is (1.34~1.39) in sodium metaaluminate and solution D in the solution C: 1；
Step 4: gel described in step 3 is placed in ultrasonic cleaner, magnetism described in step 1 is then added
Fe3O4With directed agents described in step 2, in supersonic oscillations, temperature is crystallization 2h~6h under conditions of 60 DEG C~80 DEG C, natural
Cooled and filtered, adopting and being washed with distilled water to the pH value of product is 9~10, then dry 5h under conditions of temperature is 110 DEG C
~6h obtains magnetic 4A molecular sieve.
A kind of method of above-mentioned ultrasonic wave preparation magnetism 4A molecular sieve, which is characterized in that FeCl described in step 12·
4H2O、FeCl3·6H2O、NH3·H2The additional amount of O and distilled water be respectively as follows: every liter of distilled water it is corresponding be added 18.75g~
31.25g FeCl2·4H256.25g~68.75g FeCl is added in O3·6H2125mL NH is added in O3·H2O。
The method of above-mentioned a kind of ultrasonic wave preparation magnetism 4A molecular sieve, which is characterized in that in solution A described in step 2
The mass percentage of sodium metasilicate is 35.7%~42.6%, and the mass percentage of sodium aluminate is 2.86% in the solution B
~5.4%, the mass percentage of sodium hydroxide is 11.43%~13.51%.
A kind of method of above-mentioned ultrasonic wave preparation magnetism 4A molecular sieve, which is characterized in that magnetism described in step 4
Fe3O4Additional amount be the 10%~15% of solid material quality, the additional amounts of the directed agents is the 5% of solid material quality
~10%, the quality of the solid material is the sum of Solute mass and Solute mass of solution D of solution C, and the solute of solution C is
Sodium metaaluminate and sodium hydroxide, the solute of solution D are sodium metasilicate and sodium hydroxide.
Compared with the prior art, the present invention has the following advantages:
1, the invention discloses a kind of methods using ultrasonic wave preparation magnetism 4A molecular sieve.Magnetic molecule sieve is using super
Sound wave heat plus directed agents are prepared.Ultrasonic wave is used to prepare magnetic molecule sieve by the present invention, and chemical reaction can be improved
Speed, energy conservation and environmental protection, meanwhile, directed agents are added during the preparation process, make the molecular sieve uniform particle sizes of preparation, morphological rules.
2, magnetic molecule sifter device prepared by the present invention has specific surface area high, and absorption property is strong, be easy by externally-applied magnetic field and
The advantages that reaction solution separates.
3, the present invention introduces magnetism using the magnetic 4A molecular sieve partial size of ultrasonic method synthesis about at 1.0 μm~2.0 μm
Ferriferrous oxide particles, the basic crystal structure without destruction molecular sieve obtain that crystallinity is preferable, the more uniform magnetism of granularity
4A molecular sieve.
4, the preparation and application cost of molecular sieve greatly reduces in the present invention.Added during the preparation process using ultrasonic wave
Heat substantially reduces the reaction time, reduces crystallization temperature, has saved energy consumption；Magneto separate is utilized simultaneously, improves molecular sieve
Utilization rate has very strong commercial competitiveness, will push the fast development of China's molecular sieve energetically.
5, the present invention can effectively solve the problem that in molecular sieve application and reaction solution difficulty separation problem.By adsorpting lead ion reality
It tests, the adsorption rate of magnetic molecule sieve is both greater than 95% or more, and is easy to separate with reaction solution using externally-applied magnetic field, will significantly
Promote application of the magnetic molecule sieve in absorption industry.
Invention is further described in detail with reference to the accompanying drawings and examples.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of magnetic 4A molecular sieve prepared by the embodiment of the present invention 1.
Fig. 2 is the X-ray diffractogram of magnetic 4A molecular sieve prepared by the embodiment of the present invention 1.
Fig. 3 is the infrared spectrum of magnetic 4A molecular sieve prepared by the embodiment of the present invention 1.
Specific embodiment
Embodiment 1
The present embodiment ultrasonic wave prepare magnetism 4A molecular sieve method the following steps are included:
Step 1: take a four-hole boiling flask, each oral area of flask install respectively thermometer, blender, dropping funel and
Condenser pipe；Again by NH3·H2O is added in dropping funel, is added distilled water into flask, then by FeCl2·4H2O and FeCl3·
6H2O is added in distilled water, FeCl2·4H2O、FeCl3·6H2The additional amount of O and distilled water, which is that every liter of distilled water is corresponding, to be added
25gFeCl2·4H262.5g FeCl is added in O3·6H2O；Then by persistently leading at the nozzle of condenser pipe into four-hole boiling flask
Enter nitrogen, to exclude the oxygen in flask；Blender is started later, stirs material in bottle with the stirring rate of 800r/min
It mixes, stirring while heats four-hole boiling flask, so that the instruction temperature of thermometer is maintained at 80 DEG C of constant temperature, then opens dropping liquid
NH is added dropwise into flask for funnel3·H2O, NH3·H2The additional amount of O is that 125mLNH is added in every liter of distilled water3·H2O；It drips
Continue to stir 30min with former stirring rate after finishing, obtain solidliquid mixture, after the solidliquid mixture natural cooling, utilizes
Magnet adsorbs the magnetisable material in solidliquid mixture；Adsorbed magnetisable material is washed repeatedly later, in temperature
Degree after dry 5.5h, obtains magnetic Fe under conditions of being 70 DEG C3O4；
Step 2: sodium metasilicate is dissolved in distilled water, solution A is obtained after mixing evenly, the matter of sodium metasilicate in the solution A
Measuring percentage composition is 39.2%；Sodium aluminate and sodium hydroxide are dissolved in distilled water, obtain solution B after mixing evenly, it is described molten
The mass percentage of sodium aluminate is 3.6% in liquid B, and the mass percentage of sodium hydroxide is 12.47%；Then by solution B
It is added in solution A and stirs 30min, be aged 18h later, obtain directed agents；The mass ratio of the solution A and solution B is 1.2:
1；
Step 3: sodium metaaluminate and sodium hydroxide are dissolved in distilled water, after mixing through supersonic oscillations, obtain molten
Liquid C, the concentration of sodium metaaluminate is 98g/L in the solution C, and the concentration of sodium hydroxide is 24g/L；By sodium metasilicate and sodium hydroxide
It being dissolved in distilled water, after mixing through supersonic oscillations, obtains solution D, the concentration of sodium metasilicate is 74g/L in the solution D,
The concentration of sodium hydroxide is 24g/L；Then under conditions of supersonic oscillations, solution D is dripped with the drop rate of 2.5mL/min
It is added in solution C, continues supersonic oscillations 50min after being added dropwise, obtain gel；Sodium metaaluminate and solution D in the solution C
The mass ratio of middle sodium metasilicate is 1.35: 1；
Step 4: gel described in step 3 is added in ultrasonic cleaner, magnetism described in step 1 is then added
Fe3O4With directed agents described in step 2, in supersonic oscillations, temperature is crystallization 4h under conditions of 70 DEG C, mistake after natural cooling
Filter, adopts that be washed with distilled water to the pH value of product be 10, and then dry 6h under conditions of temperature is 110 DEG C, obtains magnetism
4A molecular sieve.The magnetic Fe3O4Additional amount account for the 10% of solid material quality, the additional amount of the directed agents accounts for solid original
Expect the 5% of quality, the quality of the solid material is the sum of Solute mass and Solute mass of solution D of solution C.
The scanning electron microscope of magnetism 4A molecular sieve manufactured in the present embodiment is as shown in Figure 1, as shown in Figure 1: most magnetism
The cube shaped of rule is presented in 4A sieve particle, and crystallization degree is preferable, and partial size is more uniform.Magnetism 4A manufactured in the present embodiment points
Son sieve X-ray diffraction as shown in Fig. 2, as shown in Figure 2: magnetism 4A molecular sieve manufactured in the present embodiment by with conventional 4A molecule
The X diffraction standard map and data of sieve are compared, and can significantly be seen the high characteristic diffraction peak of 9 intensity, be shown this reality
The 4A molecular sieve for applying example preparation matches with standard diagram, and crystallization degree is preferable.Magnetism 4A molecular sieve manufactured in the present embodiment
Infrared spectrum is as shown in figure 3, from the figure 3, it may be seen that magnetic 4A molecular sieve and standard sample map that present invention ultrasonic method synthesizes have
There are much like infrared skeletal vibration bands of a spectrum.Wherein 560cm-1The absorption peak that place occurs corresponds to double Fourth Rings of magnetism 4A molecular sieve
Eigen vibration, 999cm-1The absorption peak that place occurs corresponds to oxygen-octahedron and alumina four sides in magnetism 4A molecular sieve structure skeleton
The asymmetric stretching vibration of body, 1650cm-1The absorption peak of appearance corresponds to the bending vibration of water hydroxyl, 3400cm-1What place occurred
Absorption peak corresponds to the stretching vibration of surface water hydroxyl.
Embodiment 2
The present embodiment ultrasonic wave prepare magnetism 4A molecular sieve method the following steps are included:
Step 1: take a four-hole boiling flask, each oral area of flask install respectively thermometer, blender, dropping funel and
Condenser pipe；Again by NH3·H2O is added in dropping funel, is added distilled water into flask, then by FeCl2·4H2O and FeCl3·
6H2O is added in distilled water, FeCl2·4H2O、FeCl3·6H2The additional amount of O and distilled water, which is that every liter of distilled water is corresponding, to be added
18.75gFeCl2·4H256.25g FeCl is added in O3·6H2O；Then by being held at the nozzle of condenser pipe into four-hole boiling flask
It is continuous to be passed through nitrogen, to exclude the oxygen in flask；Start blender later, make in bottle material with the stirring rate of 500r/min into
Row stirring, stirring while, heat four-hole boiling flask, so that the instruction temperature of thermometer is maintained at 75 DEG C of constant temperature, then open
NH is added dropwise into flask for dropping funel3·H2O, NH3·H2The additional amount of O is that 125mLNH is added in every liter of distilled water3·H2O；Drop
It adds and continues to stir 20min with former stirring rate after finishing, obtain solidliquid mixture, after the solidliquid mixture natural cooling,
The magnetisable material in solidliquid mixture is adsorbed using magnet；Adsorbed magnetisable material is washed repeatedly later,
Under conditions of temperature is 65 DEG C after dry 6h, magnetic Fe is obtained3O4；
Step 2: sodium metasilicate is dissolved in distilled water, solution A is obtained after mixing evenly, the matter of sodium metasilicate in the solution A
Measuring percentage composition is 35.7%；Sodium aluminate and sodium hydroxide are dissolved in distilled water, obtain solution B after mixing evenly, it is described molten
The mass percentage of sodium aluminate is 5.4% in liquid B, and the mass percentage of sodium hydroxide is 13.51%；Then by solution B
It is added in solution A and stirs 30min, be aged 18h later, obtain directed agents；The mass ratio of the solution A and solution B is 1.10:
1；
Step 3: sodium metaaluminate and sodium hydroxide are dissolved in distilled water, after mixing through supersonic oscillations, obtain molten
Liquid C, the concentration of sodium metaaluminate is 100g/L in the solution C, and the concentration of sodium hydroxide is 20g；By sodium metasilicate and sodium hydroxide
It being dissolved in distilled water, after mixing through supersonic oscillations, obtains solution D, the concentration of sodium metasilicate is 76g/L in the solution D,
The concentration of sodium hydroxide is 28g/L；Then under conditions of supersonic oscillations, solution D is dripped with the drop rate of 2.5mL/min
It is added in solution C, continues supersonic oscillations 40min after being added dropwise, obtain gel；Sodium metaaluminate and solution D in the solution C
The mass ratio of middle sodium metasilicate is 1.34: 1；
Step 4: gel described in step 3 is added in ultrasonic cleaner, magnetism described in step 1 is then added
Fe3O4With directed agents described in step 2, in supersonic oscillations, temperature is crystallization 6h under conditions of 60 DEG C, mistake after natural cooling
Filter, adopts that be washed with distilled water to the pH value of product be 10, and then dry 6h under conditions of temperature is 110 DEG C, obtains magnetism
4A molecular sieve.The magnetic Fe3O4Additional amount account for the 10% of solid material quality, the additional amount of the directed agents accounts for solid original
Expect the 10% of quality, the quality of the solid material is the sum of Solute mass and Solute mass of solution D of solution C.
By being scanned electron microscope analysis to magnetism 4A molecular sieve manufactured in the present embodiment: most magnetism 4A points
The cube shaped of rule is presented in son sieve particle, and crystallization degree is preferable, and partial size is more uniform.By to magnetism 4A manufactured in the present embodiment
The X-ray diffraction of molecular sieve is compared with the X diffraction standard map of routine 4A molecular sieve and data, can significantly see 9
The high characteristic diffraction peak of a intensity shows that 4A molecular sieve manufactured in the present embodiment matches with standard diagram, and crystallization degree is preferable.
By carrying out infrared spectrum analysis to magnetism 4A molecular sieve manufactured in the present embodiment: the magnetic that the present embodiment is synthesized with ultrasonic method
Property 4A molecular sieve and standard sample map have much like infrared skeletal vibration bands of a spectrum.Wherein 560cm-1Locate the absorption peak occurred
Corresponding to double Fourth Ring eigen vibrations of magnetic 4A molecular sieve, 999cm-1The absorption peak that place occurs corresponds to magnetism 4A molecular sieve structure
The asymmetric stretching vibration of oxygen-octahedron and aluminum-oxygen tetrahedron, 1650cm in skeleton-1The absorption peak of appearance corresponds to water hydroxyl
Bending vibration, 3400cm-1The absorption peak that place occurs corresponds to the stretching vibration of surface water hydroxyl.
Embodiment 3
The present embodiment ultrasonic wave prepare magnetism 4A molecular sieve method the following steps are included:
Step 1: take a four-hole boiling flask, each oral area of flask install respectively thermometer, blender, dropping funel and
Condenser pipe；Again by NH3·H2O is added in dropping funel, is added distilled water into flask, then by FeCl2·4H2O and FeCl3·
6H2O is added in distilled water, FeCl2·4H2O、FeCl3·6H2The additional amount of O and distilled water, which is that every liter of distilled water is corresponding, to be added
31.25gFeCl2·4H268.75g FeCl is added in O3·6H2O；Then by being held at the nozzle of condenser pipe into four-hole boiling flask
It is continuous to be passed through nitrogen, to exclude the oxygen in flask；Blender is started later, makes in bottle material with the stirring rate of 1000r/min
It is stirred, stirring while heats four-hole boiling flask, so that the instruction temperature of thermometer is maintained at 85 DEG C of constant temperature, then beats
Dropping funel is opened, NH is added dropwise into flask3·H2O, NH3·H2The additional amount of O is that 125mLNH is added in every liter of distilled water3·H2O；
Continue to stir 40min with former stirring rate after being added dropwise, solidliquid mixture is obtained, to the solidliquid mixture natural cooling
Afterwards, the magnetisable material in solidliquid mixture is adsorbed using magnet；Adsorbed magnetisable material is washed repeatedly later
It washs, under conditions of temperature is 75 DEG C after dry 6h, obtains magnetic Fe3O4；
Step 2: sodium metasilicate is dissolved in distilled water, solution A is obtained after mixing evenly, the matter of sodium metasilicate in the solution A
Measuring percentage composition is 42.6%；Sodium aluminate and sodium hydroxide are dissolved in distilled water, obtain solution B after mixing evenly, it is described molten
The mass percentage of sodium aluminate is 5.4% in liquid B, and the mass percentage of sodium hydroxide is 13.51%；Then by solution B
It is added in solution A and stirs 30min, be aged 18h later, obtain directed agents；The mass ratio of the solution A and solution B is 1.35:
1；
Step 3: sodium metaaluminate and sodium hydroxide are dissolved in distilled water, after mixing through supersonic oscillations, obtain molten
Liquid C, the concentration of sodium metaaluminate is 100g/L in the solution C, and the concentration of sodium hydroxide is 28g/L；By sodium metasilicate and hydroxide
Sodium is dissolved in distilled water, after mixing through supersonic oscillations, obtains solution D, and the concentration of sodium metasilicate is 76g/ in the solution D
L, the concentration of sodium hydroxide are 28g/L；Then under conditions of supersonic oscillations, by solution D with the drop rate of 2.5mL/min
It is added drop-wise in solution C, continues supersonic oscillations 60min after being added dropwise, obtain gel；Sodium metaaluminate and molten in the solution C
The mass ratio of sodium metasilicate is 1.39: 1 in liquid D；
Step 4: gel described in step 3 is added in ultrasonic cleaner, magnetism described in step 1 is then added
Fe3O4With directed agents described in step 2, in supersonic oscillations, temperature is crystallization 2h under conditions of 60 DEG C, mistake after natural cooling
Filter, adopts that be washed with distilled water to the pH value of product be 10, and then dry 5h under conditions of temperature is 110 DEG C, obtains magnetism
4A molecular sieve.The magnetic Fe3O4Additional amount account for the 15% of solid material quality, the additional amount of the directed agents accounts for solid original
Expect the 10% of quality, the quality of the solid material is the sum of Solute mass and Solute mass of solution D of solution C.
By being scanned electron microscope analysis to magnetism 4A molecular sieve manufactured in the present embodiment: most magnetism 4A points
The cube shaped of rule is presented in son sieve particle, and crystallization degree is preferable, and partial size is more uniform.By to magnetism 4A manufactured in the present embodiment
The X-ray diffraction of molecular sieve is compared with the X diffraction standard map of routine 4A molecular sieve and data, can significantly see 9
The high characteristic diffraction peak of a intensity shows that 4A molecular sieve manufactured in the present embodiment matches with standard diagram, and crystallization degree is preferable.
By carrying out infrared spectrum analysis to magnetism 4A molecular sieve manufactured in the present embodiment: the magnetic that the present embodiment is synthesized with ultrasonic method
Property 4A molecular sieve and standard sample map have much like infrared skeletal vibration bands of a spectrum.Wherein 560cm-1Locate the absorption peak occurred
Corresponding to double Fourth Ring eigen vibrations of magnetic 4A molecular sieve, 999cm-1The absorption peak that place occurs corresponds to magnetism 4A molecular sieve structure
The asymmetric stretching vibration of oxygen-octahedron and aluminum-oxygen tetrahedron, 1650cm in skeleton-1The absorption peak of appearance corresponds to water hydroxyl
Bending vibration, 3400cm-1The absorption peak that place occurs corresponds to the stretching vibration of surface water hydroxyl.
Embodiment 4
The present embodiment ultrasonic wave prepare magnetism 4A molecular sieve method the following steps are included:
Step 1: take a four-hole boiling flask, each oral area of flask install respectively thermometer, blender, dropping funel and
Condenser pipe；Again by NH3·H2O is added in dropping funel, is added distilled water into flask, then by FeCl2·4H2O and FeCl3·
6H2O is added in distilled water, FeCl2·4H2O、FeCl3·6H2The additional amount of O and distilled water, which is that every liter of distilled water is corresponding, to be added
31.25gFeCl2·4H268.75g FeCl is added in O3·6H2O；Then by being held at the nozzle of condenser pipe into four-hole boiling flask
It is continuous to be passed through nitrogen, to exclude the oxygen in flask；Start blender later, make in bottle material with the stirring rate of 500r/min into
Row stirring, stirring while, heat four-hole boiling flask, so that the instruction temperature of thermometer is maintained at 75 DEG C of constant temperature, then open
NH is added dropwise into flask for dropping funel3·H2O, NH3·H2The additional amount of O is that 125mLNH is added in every liter of distilled water3·H2O；Drop
It adds and continues to stir 20min with former stirring rate after finishing, obtain solidliquid mixture, after the solidliquid mixture natural cooling,
The magnetisable material in solidliquid mixture is adsorbed using magnet；Adsorbed magnetisable material is washed repeatedly later,
Under conditions of temperature is 65 DEG C after dry 5h, magnetic Fe is obtained3O4；
Step 2: sodium metasilicate is dissolved in distilled water, solution A is obtained after mixing evenly, the matter of sodium metasilicate in the solution A
Measuring percentage composition is 35.7%；Sodium aluminate and sodium hydroxide are dissolved in distilled water, obtain solution B after mixing evenly, it is described molten
The mass percentage of sodium aluminate is 2.86% in liquid B, and the mass percentage of sodium hydroxide is 11.43%；Then by solution B
It is added in solution A and stirs 30min, be aged 18h later, obtain directed agents；The mass ratio of the solution A and solution B is 1.10:
1；
Step 3: sodium metaaluminate and sodium hydroxide are dissolved in distilled water, after mixing through supersonic oscillations, obtain molten
Liquid C, the concentration of sodium metaaluminate is 96g/L in the solution C, and the concentration of sodium hydroxide is 20g/L；By sodium metasilicate and sodium hydroxide
It being dissolved in distilled water, after mixing through supersonic oscillations, obtains solution D, the concentration of sodium metasilicate is 72g/L in the solution D,
The concentration of sodium hydroxide is 20g/L；Then under conditions of supersonic oscillations, solution D is dripped with the drop rate of 2.5mL/min
It is added in solution C, continues supersonic oscillations 40min after being added dropwise, obtain gel；Sodium metaaluminate and solution D in the solution C
The mass ratio of middle sodium metasilicate is 1.36: 1；
Step 4: gel described in step 3 is added in ultrasonic cleaner, magnetism described in step 1 is then added
Fe3O4With directed agents described in step 2, in supersonic oscillations, temperature is crystallization 2h under conditions of 60 DEG C, mistake after natural cooling
Filter, adopts that be washed with distilled water to the pH value of product be 9, and then dry 5h under conditions of temperature is 110 DEG C, obtains magnetic 4A
Molecular sieve.The magnetic Fe3O4Additional amount account for the 15% of solid material quality, the additional amount of the directed agents accounts for solid material
The 5% of quality, the quality of the solid material are the sum of Solute mass and Solute mass of solution D of solution C.
By being scanned electron microscope analysis to magnetism 4A molecular sieve manufactured in the present embodiment: most magnetism 4A points
The cube shaped of rule is presented in son sieve particle, and crystallization degree is preferable, and partial size is more uniform.By to magnetism 4A manufactured in the present embodiment
The X-ray diffraction of molecular sieve is compared with the X diffraction standard map of routine 4A molecular sieve and data, can significantly see 9
The high characteristic diffraction peak of a intensity shows that 4A molecular sieve manufactured in the present embodiment matches with standard diagram, and crystallization degree is preferable.
By carrying out infrared spectrum analysis to magnetism 4A molecular sieve manufactured in the present embodiment: the magnetic that the present embodiment is synthesized with ultrasonic method
Property 4A molecular sieve and standard sample map have much like infrared skeletal vibration bands of a spectrum.Wherein 560cm-1Locate the absorption peak occurred
Corresponding to double Fourth Ring eigen vibrations of magnetic 4A molecular sieve, 999cm-1The absorption peak that place occurs corresponds to magnetism 4A molecular sieve structure
The asymmetric stretching vibration of oxygen-octahedron and aluminum-oxygen tetrahedron, 1650cm in skeleton-1The absorption peak of appearance corresponds to water hydroxyl
Bending vibration, 3400cm-1The absorption peak that place occurs corresponds to the stretching vibration of surface water hydroxyl.
Embodiment 5
The present embodiment ultrasonic wave prepare magnetism 4A molecular sieve method the following steps are included:
Step 1: take a four-hole boiling flask, each oral area of flask install respectively thermometer, blender, dropping funel and
Condenser pipe；Again by NH3·H2O is added in dropping funel, is added distilled water into flask, then by FeCl2·4H2O and FeCl3·
6H2O is added in distilled water, FeCl2·4H2O、FeCl3·6H2The additional amount of O and distilled water, which is that every liter of distilled water is corresponding, to be added
31.25gFeCl2·4H268.75g FeCl is added in O3·6H2O；Then by being held at the nozzle of condenser pipe into four-hole boiling flask
It is continuous to be passed through nitrogen, to exclude the oxygen in flask；Start blender later, make in bottle material with the stirring rate of 500r/min into
Row stirring, stirring while, heat four-hole boiling flask, so that the instruction temperature of thermometer is maintained at 85 DEG C of constant temperature, then open
NH is added dropwise into flask for dropping funel3·H2O, NH3·H2The additional amount of O is that 125mLNH is added in every liter of distilled water3·H2O；Drop
It adds and continues to stir 40min with former stirring rate after finishing, obtain solidliquid mixture, after the solidliquid mixture natural cooling,
The magnetisable material in solidliquid mixture is adsorbed using magnet；Adsorbed magnetisable material is washed repeatedly later,
Under conditions of temperature is 65 DEG C after dry 6h, magnetic Fe is obtained3O4；
Step 2: sodium metasilicate is dissolved in distilled water, solution A is obtained after mixing evenly, the matter of sodium metasilicate in the solution A
Measuring percentage composition is 42.6%；Sodium aluminate and sodium hydroxide are dissolved in distilled water, obtain solution B after mixing evenly, it is described molten
The mass percentage of sodium aluminate is 2.86% in liquid B, and the mass percentage of sodium hydroxide is 13.51%；Then by solution B
It is added in solution A and stirs 30min, be aged 18h later, obtain directed agents；The mass ratio of the solution A and solution B is 1.10:
1；
Step 3: sodium metaaluminate and sodium hydroxide are dissolved in distilled water, after mixing through supersonic oscillations, obtain molten
Liquid C, the concentration of sodium metaaluminate is 100g/L in the solution C, and the concentration of sodium hydroxide is 20g/L；By sodium metasilicate and hydroxide
Sodium is dissolved in distilled water, after mixing through supersonic oscillations, obtains solution D, and the concentration of sodium metasilicate is 76g/ in the solution D
L, the concentration of sodium hydroxide are 20g/L；Then under conditions of supersonic oscillations, by solution D with the drop rate of 2.5mL/min
It is added drop-wise in solution C, continues supersonic oscillations 40min after being added dropwise, obtain gel；Sodium metaaluminate and molten in the solution C
The mass ratio of sodium metasilicate is 1.37: 1 in liquid D；
Step 4: gel described in step 3 is added in ultrasonic cleaner, magnetism described in step 1 is then added
Fe3O4With directed agents described in step 2, in supersonic oscillations, temperature is crystallization 6h under conditions of 60 DEG C, mistake after natural cooling
Filter, adopts that be washed with distilled water to the pH value of product be 9, and then dry 6h under conditions of temperature is 110 DEG C, obtains magnetic 4A
Molecular sieve.The magnetic Fe3O4Additional amount account for the 10% of solid material quality, the additional amount of the directed agents accounts for solid material
The 5% of quality, the quality of the solid material are the sum of Solute mass and Solute mass of solution D of solution C.
By being scanned electron microscope analysis to magnetism 4A molecular sieve manufactured in the present embodiment: most magnetism 4A points
The cube shaped of rule is presented in son sieve particle, and crystallization degree is preferable, and partial size is more uniform.By to magnetism 4A manufactured in the present embodiment
The X-ray diffraction of molecular sieve is compared with the X diffraction standard map of routine 4A molecular sieve and data, can significantly see 9
The high characteristic diffraction peak of a intensity shows that 4A molecular sieve manufactured in the present embodiment matches with standard diagram, and crystallization degree is preferable.
By carrying out infrared spectrum analysis to magnetism 4A molecular sieve manufactured in the present embodiment: the magnetic that the present embodiment is synthesized with ultrasonic method
Property 4A molecular sieve and standard sample map have much like infrared skeletal vibration bands of a spectrum.Wherein 560cm-1Locate the absorption peak occurred
Corresponding to double Fourth Ring eigen vibrations of magnetic 4A molecular sieve, 999cm-1The absorption peak that place occurs corresponds to magnetism 4A molecular sieve structure
The asymmetric stretching vibration of oxygen-octahedron and aluminum-oxygen tetrahedron, 1650cm in skeleton-1The absorption peak of appearance corresponds to water hydroxyl
Bending vibration, 3400cm-1The absorption peak that place occurs corresponds to the stretching vibration of surface water hydroxyl.
The above is only presently preferred embodiments of the present invention, is not intended to limit the invention in any way.It is all according to invention skill
Art any simple modification, change and equivalence change substantially to the above embodiments, still fall within technical solution of the present invention
Protection scope in.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610993852.4A CN106517355B (en) | 2016-11-11 | 2016-11-11 | A kind of method of ultrasonic wave preparation magnetism 4A molecular sieve |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610993852.4A CN106517355B (en) | 2016-11-11 | 2016-11-11 | A kind of method of ultrasonic wave preparation magnetism 4A molecular sieve |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106517355A CN106517355A (en) | 2017-03-22 |
| CN106517355B true CN106517355B (en) | 2019-01-04 |
Family
ID=58350743
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610993852.4A Expired - Fee Related CN106517355B (en) | 2016-11-11 | 2016-11-11 | A kind of method of ultrasonic wave preparation magnetism 4A molecular sieve |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106517355B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107149924A (en) * | 2017-06-15 | 2017-09-12 | 福州大学 | A kind of preparation of magnetic nanometer adsorbent and its application in compound wastewater processing |
| CN107311195A (en) * | 2017-07-31 | 2017-11-03 | 西安科技大学 | A kind of preparation method and application of magnetic 5A molecular sieves |
| CN110102255B (en) * | 2019-04-03 | 2021-10-19 | 广东工业大学 | A kind of magnetic carbon nanotube composite material doped with molecular sieve and its preparation method and application |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1699171A (en) * | 2005-05-12 | 2005-11-23 | 山东铝业股份有限公司 | Manufacturing process of 4A type molecular sieve primary powder with low bulk density |
| CN100413783C (en) * | 2006-06-06 | 2008-08-27 | 河北工业大学 | 4A type zeolite molecular sieve and preparation method thereof |
| CN102936019A (en) * | 2012-11-09 | 2013-02-20 | 合肥工业大学 | Method for preparing magnetic 4A molecular sieve by using kaolin |
-
2016
- 2016-11-11 CN CN201610993852.4A patent/CN106517355B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN106517355A (en) | 2017-03-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106517355B (en) | A kind of method of ultrasonic wave preparation magnetism 4A molecular sieve | |
| CN100434364C (en) | Synthesis of Zeolite 4A by Low-temperature Alkali Fusion of Kaolin | |
| JP5224223B1 (en) | Method for producing cation sorbent | |
| CN104291349A (en) | Method for preparing P type molecular sieve by using coal ash as raw material | |
| CN112811435B (en) | A method for synthesizing analcime by microwave hydrothermal crystallization of coal gangue | |
| CN105126763B (en) | A kind of preparation method of attapulgite composite material for adsorbing separation azeotropic mixture | |
| CN101406825A (en) | Method for synthesizing 4A molecular sieve drier using kaoline | |
| CN104888705B (en) | The preparation method of magnetic iron oxide/bagasse active carbon | |
| Chen et al. | Magnetic solid-phase extraction of proteins based on hydroxy functional ionic liquid-modified magnetic nanoparticles | |
| CN117732255B (en) | Preparation method of LTA molecular sieve nanocrystalline mixed matrix membrane | |
| CN109718825A (en) | Microballoon Silicate-1 molecular sieve catalyst and preparation method thereof and the method for preparing caprolactam | |
| CN109718826A (en) | Microballoon Silicate-1 molecular sieve catalyst and preparation method thereof and the method for preparing caprolactam | |
| CN109534354A (en) | A kind of synthetic method of SSZ-13 molecular sieve | |
| CN110451520B (en) | A magnetic molecular sieve/straw carbon composite material and its preparation method and application | |
| CN106902747B (en) | A kind of amidoxime mesoporous silica microsphere adsorbent and preparation method thereof | |
| CN103285828A (en) | Preparation method of magnesium oxide adsorbent capable of absorbing azo dyes and being recycled and regenerated | |
| CN107311195A (en) | A kind of preparation method and application of magnetic 5A molecular sieves | |
| CN108726534B (en) | Preparation method of micro-mesoporous ZSM-5 molecular sieve | |
| CN102755880B (en) | Method for preparing high-purity silica packing through sol-gel process | |
| CN101497025B (en) | Method for preparing active carbon-aluminosilicate composite adsorbent with oil shale as raw material | |
| CN109675521A (en) | A kind of graphene oxide-gadolinium hydroxide composite material, preparation method and applications | |
| CN109464981A (en) | Method for preparing magnetic nanomaterial, and method for separating boron isotopes by using the magnetic nanomaterial as a stationary phase in a simulated moving bed | |
| CN104291348B (en) | Method for preparing novel analcite by adding spatial steric hindering agent | |
| CN111085259A (en) | Silicon oxide and SAPO-34 zeolite composite material and synthetic method thereof | |
| CN108862342A (en) | A kind of modified gangue preparation γ-Al2O3The method of nanometer sheet |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20190104 Termination date: 20201111 |