CN108892151A - A kind of flyash ZSM-5 molecular sieve and preparation method thereof - Google Patents
A kind of flyash ZSM-5 molecular sieve and preparation method thereof Download PDFInfo
- Publication number
- CN108892151A CN108892151A CN201810677694.0A CN201810677694A CN108892151A CN 108892151 A CN108892151 A CN 108892151A CN 201810677694 A CN201810677694 A CN 201810677694A CN 108892151 A CN108892151 A CN 108892151A
- Authority
- CN
- China
- Prior art keywords
- flyash
- zsm
- molecular sieve
- preparation
- roasting
- 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.)
- Pending
Links
Classifications
-
- 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
- C01B39/36—Pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11
- C01B39/38—Type ZSM-5
- C01B39/40—Type ZSM-5 using at least one organic template directing agent
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B37/00—Compounds having molecular sieve properties but not having base-exchange properties
- C01B37/005—Silicates, i.e. so-called metallosilicalites or metallozeosilites
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention belongs to a kind of ZSM-5 molecular sieves to synthesize field, and in particular to a kind of flyash ZSM-5 molecular sieve and preparation method thereof.The present invention using flyash as raw material, by its with natrium carbonicum calcinatum it is baking mixed after, dissolve and mixed with the water and sodium hydroxide of natrium carbonicum calcinatum appropriate volume, supplement a certain amount of aluminum sulfate, template, silica solution, obtain ZSM-5 molecular sieve after assisting subsequent crystallization.Synthesis process step of the invention is simple, solves solid waste flyash and brings the wasting of resources and environmental problem, has significant economic value and social benefit.
Description
Technical field
The invention belongs to a kind of ZSM-5 molecular sieve fields, and in particular to synthesize ZSM-5 molecular sieve with industrial waste flyash
Method, i.e., a kind of flyash ZSM-5 molecular sieve and preparation method thereof.
Background technique
China is in the world biggish " ash discharge state " that flyash is mainly derived from the thermal power generation using coal as main fuel
Factory and the power boiler of large industrial enterprise etc., Chinese Thermal Power Generation Industry 1 year discharge flyash in contain 358.75 tons of cadmium, chromium
10054.25 tons, 9410 tons of arsenic, 4.25 tons of mercury, 5345.5 tons of lead, about 2.5 ten thousand tons in total.These harmful substances are to natural environment
Huge threat is all constituted with human health.In order to preferably protect environment, the recycling treatment and comprehensive utilization of flyash
Problem causes the extensive concern of people, also becomes the important research class in China environmental protection and renewable energy development field
Topic.About the comprehensive development and utilization of flyash, early in early 20th century, the U.S. has found that the characteristics of Ash Utilization utilizes simultaneously
It begins one's study to it.After World War II, the development of capitalist country industrial sector is swift and violent, the slag after having discharged a large amount of coal burnings
Dregs is taken seriously the comprehensive utilization of fly ash.Compared to some European countries, Chinese starts late, I
State is a few one of country used coal as its main energy source in the world, and some local environment problems is caused to emerge one after another.China
Utilization of fly ash originates in the 1950s, and setting specialized agency the sixties[9].It is comprehensive with regard to domestic and international flyash at present
Close utilize the case where from the point of view of, flyash construction material, engineering construction, chemical industry, agricultural, in terms of application
Technical comparing is mature.
Because its own property and its chemical component can produce the ZSM-5 molecular sieve containing high silicon ingredient, and industrially produce
The raw material of ZSM-5 molecular sieve is the industrial chemicals and all kinds of templates of silicon source, silicon source mostly, higher cost be presently, there are one
A major issue.This project uses flyash for raw material, obtains silicon source after classification processing, the core competitive power that can not only be improved
Power can also solve the problem of environmental pollution of certain limit, and the shortage of resource is effectively relieved, and to electric power industry development is accelerated, promote
Into the rapid development of national economy, there is especially important meaning.
Summary of the invention
The invention belongs to a kind of ZSM-5 molecular sieves to synthesize field, and in particular to a kind of standby with industrial waste coal ash for manufacturing
The method of ZSM-5 molecular sieve.The present invention using flyash as raw material, by its with natrium carbonicum calcinatum it is baking mixed after, dissolve and and nothing
The water and sodium hydroxide of aqueous sodium carbonate appropriate volume mix, and supplement a certain amount of aluminum sulfate, template, silica solution, after auxiliary
ZSM-5 molecular sieve is obtained after continuous crystallization.Synthesis process step of the invention is simple, solves solid waste flyash and brings resource
Waste and environmental problem have significant economic value and social benefit.
The present invention will be realized using following technical scheme：
(1) 200 meshes are crossed after grinding flyash, are taken out after the flyash heating after taking sieving, by the fine coal after roasting
Distilled water, stirring is added in ash, and heating washing filters to get filtrate and filter residue, by after drying filter residue and activator Na2CO3 with mixed
Heating roasting is closed, crushes to obtain activating fly ash after cooling；The flyash of activation is filtered after middle addition acid solution, residue washing
It to neutrality, is taken out after dry, obtains silicic acid precipitating
(2) TPAOH in molar ratio:H2SiO3 (silicic acid precipitating):SiO2:H2O:Al2O3=1:x:6:571:0.005, x=
0.006-0.06 supplements tetrapropylammonium hydroxide, silicic acid precipitating, silicon source and distilled water, is mixed, is washed till neutrality after crystallization, does
Flyash ZSM-5 molecular sieve is obtained after dry.
Wherein, the mass ratio of the flyash after drying and activator Na2CO3 are 1:1-1:2；Flyash after the sieving
Maturing temperature is that 800 DEG C of calcining times are 2h；Flyash after the roasting is heated to 75 DEG C after adding water, washes 0-3h；It will do
Heating maturing temperature is 840 DEG C after filter residue after dry is mixed with activator, calcining time 3h；Drying temperature described in step 1 is
80-120℃
Wherein, the acid solution is hydrochloric acid solution, solution concentration 1-5mol/L.
Wherein, crystallization temperature is 120-210 DEG C.
Wherein, crystallization time 12-48h.
Wherein, source of aluminium is one or more of aluminium oxide, aluminium hydroxide, sodium aluminate
The beneficial effects of the invention are as follows：A kind of method with industrial waste coal ash for manufacturing for ZSM-5 molecular sieve is developed, is obtained
ZSM-5 molecular sieve better crystallinity degree, specific surface area is high, Kong Rong great and be multistage hollow structure, while it is useless to also solve solid
The wasting of resources and bring environmental problem of object have certain economic benefit and social value.
Detailed description of the invention
Fig. 1：ZSM-5 molecular sieve XRD diagram is synthesized under different silicic acid additional amounts.
Fig. 2：ZSM-5 molecular sieve XRD diagram is synthesized under different crystallization temperatures.
Fig. 3：ZSM-5 molecular sieve XRD diagram is synthesized under different crystallization times.
Fig. 4：The N2 adsorption-desorption curve of sample in embodiment 1.
As can be seen from Figure, suitable silicic acid additional amount, crystallization time and crystallization temperature are controlled, can just be crystallized
High ZSM-5 molecular sieve is spent, with high-specific surface area and hierarchical porous structure.
Specific embodiment
Technical solution of the invention is further illustrated combined with specific embodiments below, these embodiments should not be understood as
It is the limitation to technical solution.
Embodiment 1：ZSM-5 molecular sieve is prepared according to following steps
Flyash is ground into a period of time and crosses 200 meshes, the flyash after taking a certain amount of sieving is put into Muffle stove heating
It being taken out after to 800 DEG C of roasting 2h, the distilled water of solid-to-liquid ratio 1g/20mL is added in the flyash after taking-up, and stirring is heated to 75 DEG C,
Stop heating and stirring after washing 3h, filters to get filtrate and filter residue, filter residue take out after dry 2h in 120 DEG C of baking ovens, take certain
Flyash sample after the washing of amount.Using natrium carbonicum calcinatum as activator, flyash and Na2CO3With mass ratio 1:1 mixing is equal
It is put into porcelain crucible after even, is placed in Muffle furnace and is heated to 840 DEG C of roasting 3h, taken out after cooling, material is light green color, powder at this time
Activating fly ash is obtained after broken.The product of roasting of activation is put into beaker, the hydrochloric acid solution of 3mol/L is added while stirring, wait fill
It filters after dividing acidleach, residue washing to neutrality, is taken out after dry at 120 DEG C, obtain silicic acid precipitating.TPAOH in molar ratio:
(silicic acid precipitating):SiO2:H2O:Al2O3=1:0.012:6:571:0.005, supplement tetrapropylammonium hydroxide, silicic acid precipitating, sulphur
1h is mixed in sour aluminium and distilled water, and setting silicic acid additional amount is respectively 0.5,0.2,0.1,0.05g, is put into stainless steel reaction
For 24 hours, taking-up is washed till neutrality to crystallization at 180 DEG C in kettle, obtains sample after dry.Obtain the N of sample2Adsorption-desorption curve is such as
Shown in Fig. 4.
Embodiment 2：ZSM-5 molecular sieve is prepared according to following steps
Flyash is ground into a period of time and crosses 200 meshes, the flyash after taking a certain amount of sieving is put into Muffle stove heating
It being taken out after to 800 DEG C of roasting 2h, the distilled water of solid-to-liquid ratio 1g/20mL is added in the flyash after taking-up, and stirring is heated to 75 DEG C,
Stop heating and stirring after washing 3h, filters to get filtrate and filter residue, filter residue take out after dry 2h in 120 DEG C of baking ovens, take certain
Flyash sample after the washing of amount.Using natrium carbonicum calcinatum as activator, flyash and Na2CO3With mass ratio 1:1 mixing is equal
It is put into porcelain crucible after even, is placed in Muffle furnace and is heated to 840 DEG C of roasting 3h, taken out after cooling, material is light green color, powder at this time
Activating fly ash is obtained after broken.The product of roasting of activation is put into beaker, the hydrochloric acid solution of 3mol/L is added while stirring, wait fill
It filters after dividing acidleach, residue washing to neutrality, is taken out after dry at 120 DEG C, obtain silicic acid precipitating.TPAOH in molar ratio:
(silicic acid precipitating):SiO2:H2O:Al2O3=1:0.006:6:571:0.005, supplement tetrapropylammonium hydroxide, silicic acid precipitating, sulphur
1h is mixed in sour aluminium and distilled water, and being put into stainless steel cauldron the crystallization at 180 DEG C, for 24 hours, taking-up is washed till neutrality, dry
After obtain sample.
Embodiment 3：ZSM-5 molecular sieve is prepared according to following steps
Flyash is ground into a period of time and crosses 200 meshes, the flyash after taking a certain amount of sieving is put into Muffle stove heating
It being taken out after to 800 DEG C of roasting 2h, the distilled water of solid-to-liquid ratio 1g/20mL is added in the flyash after taking-up, and stirring is heated to 75 DEG C,
Stop heating and stirring after washing 3h, filters to get filtrate and filter residue, filter residue take out after dry 2h in 120 DEG C of baking ovens, take certain
Flyash sample after the washing of amount.Using natrium carbonicum calcinatum as activator, flyash and Na2CO3With mass ratio 1:1 mixing is equal
It is put into porcelain crucible after even, is placed in Muffle furnace and is heated to 840 DEG C of roasting 3h, taken out after cooling, material is light green color, powder at this time
Activating fly ash is obtained after broken.The product of roasting of activation is put into beaker, the hydrochloric acid solution of 1mol/L is added while stirring, wait fill
It filters after dividing acidleach, residue washing to neutrality, is taken out after dry at 120 DEG C, obtain silicic acid precipitating.TPAOH in molar ratio:
(silicic acid precipitating):SiO2:H2O:Al2O3=1:0.024:6:571:0.005, supplement tetrapropylammonium hydroxide, silicic acid precipitating, sulphur
1h is mixed in sour aluminium and distilled water, and being put into stainless steel cauldron the crystallization at 180 DEG C, for 24 hours, taking-up is washed till neutrality, dry
After obtain sample.
Embodiment 4：ZSM-5 molecular sieve is prepared according to following steps
Flyash is ground into a period of time and crosses 200 meshes, the flyash after taking a certain amount of sieving is put into Muffle stove heating
It being taken out after to 800 DEG C of roasting 2h, the distilled water of solid-to-liquid ratio 1g/20mL is added in the flyash after taking-up, and stirring is heated to 75 DEG C,
Stop heating and stirring after washing 3h, filters to get filtrate and filter residue, filter residue take out after dry 2h in 120 DEG C of baking ovens, take certain
Flyash sample after the washing of amount.Using natrium carbonicum calcinatum as activator, flyash and Na2CO3With mass ratio 1:1 mixing is equal
It is put into porcelain crucible after even, is placed in Muffle furnace and is heated to 840 DEG C of roasting 3h, taken out after cooling, material is light green color, powder at this time
Activating fly ash is obtained after broken.The product of roasting of activation is put into beaker, the hydrochloric acid solution of 3mol/L is added while stirring, wait fill
It filters after dividing acidleach, residue washing to neutrality, is taken out after dry at 120 DEG C, obtain silicic acid precipitating.TPAOH in molar ratio:
(silicic acid precipitating):SiO2:H2O:Al2O3=1:0.06:6:571:0.005, supplement tetrapropylammonium hydroxide, silicic acid precipitating, sulfuric acid
1h is mixed in aluminium and distilled water, and being put into stainless steel cauldron the crystallization at 180 DEG C, for 24 hours, taking-up is washed till neutrality, after dry
Obtain sample.
Embodiment 5：ZSM-5 molecular sieve is prepared according to following steps
Flyash is ground into a period of time and crosses 200 meshes, the flyash after taking a certain amount of sieving is put into Muffle stove heating
It being taken out after to 800 DEG C of roasting 2h, the distilled water of solid-to-liquid ratio 1g/20mL is added in the flyash after taking-up, and stirring is heated to 75 DEG C,
Stop heating and stirring after washing 3h, filters to get filtrate and filter residue, filter residue take out after dry 2h in 120 DEG C of baking ovens, take certain
Flyash sample after the washing of amount.Using natrium carbonicum calcinatum as activator, flyash and Na2CO3With mass ratio 1:1 mixing is equal
It is put into porcelain crucible after even, is placed in Muffle furnace and is heated to 840 DEG C of roasting 3h, taken out after cooling, material is light green color, powder at this time
Activating fly ash is obtained after broken.The product of roasting of activation is put into beaker, the hydrochloric acid solution of 3mol/L is added while stirring, wait fill
It filters after dividing acidleach, residue washing to neutrality, is taken out after dry at 120 DEG C, obtain silicic acid precipitating.TPAOH in molar ratio:
(silicic acid precipitating):SiO2:H2O:Al2O3=1:0.012:6:571:0.005, supplement tetrapropylammonium hydroxide, silicic acid precipitating, sulphur
1h is mixed in sour aluminium and distilled water, and being put into stainless steel cauldron the crystallization at 120 DEG C, for 24 hours, taking-up is washed till neutrality, dry
After obtain sample.
Embodiment 6：ZSM-5 molecular sieve is prepared according to following steps
Flyash is ground into a period of time and crosses 200 meshes, the flyash after taking a certain amount of sieving is put into Muffle stove heating
It being taken out after to 800 DEG C of roasting 2h, the distilled water of solid-to-liquid ratio 1g/20mL is added in the flyash after taking-up, and stirring is heated to 75 DEG C,
Stop heating and stirring after washing 3h, filters to get filtrate and filter residue, filter residue take out after dry 2h in 120 DEG C of baking ovens, take certain
Flyash sample after the washing of amount.Using natrium carbonicum calcinatum as activator, flyash and Na2CO3With mass ratio 1:1 mixing is equal
It is put into porcelain crucible after even, is placed in Muffle furnace and is heated to 840 DEG C of roasting 3h, taken out after cooling, material is light green color, powder at this time
Activating fly ash is obtained after broken.The product of roasting of activation is put into beaker, the hydrochloric acid solution of 3mol/L is added while stirring, wait fill
It filters after dividing acidleach, residue washing to neutrality, is taken out after dry at 120 DEG C, obtain silicic acid precipitating.TPAOH in molar ratio:
(silicic acid precipitating):SiO2:H2O:Al2O3=1:0.012:6:571:0.005, supplement tetrapropylammonium hydroxide, silicic acid precipitating, sulphur
1h is mixed in sour aluminium and distilled water, and being put into stainless steel cauldron the crystallization at 150 DEG C, for 24 hours, taking-up is washed till neutrality, dry
After obtain sample.
Embodiment 7：ZSM-5 molecular sieve is prepared according to following steps
Flyash is ground into a period of time and crosses 200 meshes, the flyash after taking a certain amount of sieving is put into Muffle stove heating
It being taken out after to 800 DEG C of roasting 2h, the distilled water of solid-to-liquid ratio 1g/20mL is added in the flyash after taking-up, and stirring is heated to 75 DEG C,
Stop heating and stirring after washing 3h, filters to get filtrate and filter residue, filter residue take out after dry 2h in 120 DEG C of baking ovens, take certain
Flyash sample after the washing of amount.Using natrium carbonicum calcinatum as activator, flyash and Na2CO3With mass ratio 1:1 mixing is equal
It is put into porcelain crucible after even, is placed in Muffle furnace and is heated to 840 DEG C of roasting 3h, taken out after cooling, material is light green color, powder at this time
Activating fly ash is obtained after broken.The product of roasting of activation is put into beaker, the hydrochloric acid solution of 5mol/L is added while stirring, wait fill
It filters after dividing acidleach, residue washing to neutrality, is taken out after dry at 120 DEG C, obtain silicic acid precipitating.TPAOH in molar ratio:
(silicic acid precipitating):SiO2:H2O:Al2O3=1:0.012:6:571:0.005, supplement tetrapropylammonium hydroxide, silicic acid precipitating, sulphur
1h is mixed in sour aluminium and distilled water, and being put into stainless steel cauldron the crystallization at 210 DEG C, for 24 hours, taking-up is washed till neutrality, dry
After obtain sample.
Embodiment 8：ZSM-5 molecular sieve is prepared according to following steps
Flyash is ground into a period of time and crosses 200 meshes, the flyash after taking a certain amount of sieving is put into Muffle stove heating
It being taken out after to 800 DEG C of roasting 2h, the distilled water of solid-to-liquid ratio 1g/20mL is added in the flyash after taking-up, and stirring is heated to 75 DEG C,
Stop heating and stirring after washing 3h, filters to get filtrate and filter residue, filter residue take out after dry 2h in 120 DEG C of baking ovens, take certain
Flyash sample after the washing of amount.Using natrium carbonicum calcinatum as activator, flyash and Na2CO3With mass ratio 1:1 mixing is equal
It is put into porcelain crucible after even, is placed in Muffle furnace and is heated to 840 DEG C of roasting 3h, taken out after cooling, material is light green color, powder at this time
Activating fly ash is obtained after broken.The product of roasting of activation is put into beaker, the hydrochloric acid solution of 5mol/L is added while stirring, wait fill
It filters after dividing acidleach, residue washing to neutrality, is taken out after dry at 120 DEG C, obtain silicic acid precipitating.TPAOH in molar ratio:
(silicic acid precipitating):SiO2:H2O:Al2O3=1:0.024:6:571:0.005, supplement tetrapropylammonium hydroxide, silicic acid precipitating, sulphur
1h is mixed in sour aluminium and distilled water, is put into stainless steel cauldron the crystallization 12h at 180 DEG C, and taking-up is washed till neutrality, dry
After obtain sample.
Embodiment 9：ZSM-5 molecular sieve is prepared according to following steps
Flyash is ground into a period of time and crosses 200 meshes, the flyash after taking a certain amount of sieving is put into Muffle stove heating
It being taken out after to 800 DEG C of roasting 2h, the distilled water of solid-to-liquid ratio 1g/20mL is added in the flyash after taking-up, and stirring is heated to 75 DEG C,
Stop heating and stirring after washing 3h, filters to get filtrate and filter residue, filter residue take out after dry 2h in 120 DEG C of baking ovens, take certain
Flyash sample after the washing of amount.Using natrium carbonicum calcinatum as activator, flyash and Na2CO3With mass ratio 1:1 mixing is equal
It is put into porcelain crucible after even, is placed in Muffle furnace and is heated to 840 DEG C of roasting 3h, taken out after cooling, material is light green color, powder at this time
Activating fly ash is obtained after broken.The product of roasting of activation is put into beaker, the hydrochloric acid solution of 3mol/L is added while stirring, wait fill
It filters after dividing acidleach, residue washing to neutrality, is taken out after dry at 120 DEG C, obtain silicic acid precipitating.TPAOH in molar ratio:
(silicic acid precipitating):SiO2:H2O:Al2O3=1:0.012:6:571:0.005, supplement tetrapropylammonium hydroxide, silicic acid precipitating, sulphur
1h is mixed in sour aluminium and distilled water, is put into stainless steel cauldron the crystallization 36h at 180 DEG C, and taking-up is washed till neutrality, dry
After obtain sample.
Embodiment 10：ZSM-5 molecular sieve is prepared according to following steps
Flyash is ground into a period of time and crosses 200 meshes, the flyash after taking a certain amount of sieving is put into Muffle stove heating
It being taken out after to 800 DEG C of roasting 2h, the distilled water of solid-to-liquid ratio 1g/20mL is added in the flyash after taking-up, and stirring is heated to 75 DEG C,
Stop heating and stirring after washing 3h, filters to get filtrate and filter residue, filter residue take out after dry 2h in 120 DEG C of baking ovens, take certain
Flyash sample after the washing of amount.Using natrium carbonicum calcinatum as activator, flyash and Na2CO3With mass ratio 1:1 mixing is equal
It is put into porcelain crucible after even, is placed in Muffle furnace and is heated to 840 DEG C of roasting 3h, taken out after cooling, material is light green color, powder at this time
Activating fly ash is obtained after broken.The product of roasting of activation is put into beaker, the hydrochloric acid solution of 3mol/L is added while stirring, wait fill
It filters after dividing acidleach, residue washing to neutrality, is taken out after dry at 120 DEG C, obtain silicic acid precipitating.TPAOH in molar ratio:
(silicic acid precipitating):SiO2:H2O:Al2O3=1:0.012:6:571:0.005, supplement tetrapropylammonium hydroxide, silicic acid precipitating, sulphur
1h is mixed in sour aluminium and distilled water, is put into stainless steel cauldron the crystallization 48h at 180 DEG C, and taking-up is washed till neutrality, dry
After obtain sample.
As can be seen from the above embodiments, the present invention develops a kind of side with industrial waste coal ash for manufacturing for ZSM-5 molecular sieve
Method solves the wasting of resources and bring environmental problem of solid waste, has apparent economy and environmental benefit.
Technical solution of the present invention is not limited to examples detailed above, and the other embodiments obtained according to the technique and scheme of the present invention are equal
It should fall into claim of the invention.
Claims (7)
1. a kind of preparation method of flyash ZSM-5 molecular sieve, which is characterized in that include the following steps：
(1) 200 meshes are crossed after grinding flyash, take out after the flyash heating after taking sieving, the flyash after roasting is added
Enter distilled water, stir, heating washing filters to get filtrate and filter residue, by the filter residue and activator Na after drying2CO3With Hybrid Heating
Roasting crushes to obtain activating fly ash after cooling；The flyash of activation is filtered after middle addition acid solution, residue washing is into
Property, it is taken out after dry, obtains silicic acid precipitating；
(2) TPAOH in molar ratio:H2SiO3(silicic acid precipitating):SiO2:H2O:Al2O3=1:x:6:571:0.005, x=0.006-
0.06 supplement tetrapropylammonium hydroxide, silicic acid precipitating, silicon source and distilled water, are mixed, and neutrality is washed till after crystallization, is obtained after dry
Obtain flyash ZSM-5 molecular sieve.
2. the preparation method of flyash ZSM-5 molecular sieve according to claim 1, it is characterised in that：It is filtered described in step 1
Flyash and activator Na after drying2CO3Mass ratio be 1:1-1:2；Flyash maturing temperature after the sieving is 700-
1000 DEG C of calcining times are 1-5h；Flyash after the roasting is heated to 60-80 DEG C after adding water, washes 0-3h；After dry
Filter residue mixed with activator after heating maturing temperature be 800-850 DEG C, calcining time 2-4h；Drying temperature described in step 1
It is 80-120 DEG C.
3. the preparation method of flyash ZSM-5 molecular sieve according to claim 1, it is characterised in that：In the step 1, institute
Stating acid solution is hydrochloric acid solution, solution concentration 1-5mol/L.
4. the preparation method of flyash ZSM-5 molecular sieve according to claim 1, it is characterised in that：Crystallization described in step 2
Temperature is 120-210 DEG C.
5. the preparation method of flyash ZSM-5 molecular sieve according to claim 1, it is characterised in that：Crystallization described in step 2
Time is 12-48h.
6. the preparation method of flyash ZSM-5 molecular sieve according to claim 1, it is characterised in that：Silicon source described in step 2 is
One or more of aluminium oxide, aluminium hydroxide, sodium aluminate.
7. a kind of ZSM-5 preparation of the preparation method preparation of -6 any flyash ZSM-5 molecular sieves according to claim 1
Molecular sieve.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810677694.0A CN108892151A (en) | 2018-06-27 | 2018-06-27 | A kind of flyash ZSM-5 molecular sieve and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810677694.0A CN108892151A (en) | 2018-06-27 | 2018-06-27 | A kind of flyash ZSM-5 molecular sieve and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108892151A true CN108892151A (en) | 2018-11-27 |
Family
ID=64346514
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810677694.0A Pending CN108892151A (en) | 2018-06-27 | 2018-06-27 | A kind of flyash ZSM-5 molecular sieve and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108892151A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109621903A (en) * | 2019-01-31 | 2019-04-16 | 上海交通大学 | A method of preparing sludge base charcoal zeolite functional material |
| CN109824059A (en) * | 2019-03-13 | 2019-05-31 | 东北大学 | A kind of preparation method of ZSM-5 zeolite |
| CN109879295A (en) * | 2019-04-25 | 2019-06-14 | 太原理工大学 | A kind of ZSM-5 molecular sieve |
| CN110156044A (en) * | 2019-06-14 | 2019-08-23 | 河南理工大学 | A kind of preparation method of no sodium fly ash base ZSM-5 molecular sieve |
| CN111039301A (en) * | 2019-12-31 | 2020-04-21 | 青岛科技大学 | Method for preparing hierarchical pore ZSM-5 molecular sieve by using fly ash |
| CN114212799A (en) * | 2021-12-21 | 2022-03-22 | 黑龙江省能源环境研究院 | Coal ash pretreatment method for molecular sieve preparation |
| CN114506856A (en) * | 2022-01-21 | 2022-05-17 | 贵州理工学院 | Method for preparing ZSM-5 molecular sieve from industrial silicon waste |
| CN115770609A (en) * | 2022-11-17 | 2023-03-10 | 华电电力科学研究院有限公司 | Preparation method of fly ash-based Fe/ZSM-5 mesoporous molecular sieve catalyst |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103435064A (en) * | 2013-08-20 | 2013-12-11 | 东北石油大学 | Method for preparing nano-scale ZSM-5 molecular sieve by using coal ash |
| CN103787366A (en) * | 2014-01-26 | 2014-05-14 | 淮南师范学院 | Preparation method of low-cost ZSM-5 type zeolite molecular sieve, and application thereof |
| CN104056652A (en) * | 2013-03-22 | 2014-09-24 | 中国石油化工股份有限公司 | Core-shell ZSM-5 molecular sieve microsphere catalyst |
| CN106784917A (en) * | 2016-12-16 | 2017-05-31 | 哈尔滨工业大学深圳研究生院 | A kind of method of modifying of the PEM for all-vanadium flow battery |
| WO2017221192A1 (en) * | 2016-06-23 | 2017-12-28 | University Of The Western Cape | Process for production of high silica content zeolite from fly ash |
| CN107697927A (en) * | 2017-11-14 | 2018-02-16 | 江苏理工学院 | A kind of preparation method using flyash as the NaA molecular sieve of raw material |
-
2018
- 2018-06-27 CN CN201810677694.0A patent/CN108892151A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104056652A (en) * | 2013-03-22 | 2014-09-24 | 中国石油化工股份有限公司 | Core-shell ZSM-5 molecular sieve microsphere catalyst |
| CN103435064A (en) * | 2013-08-20 | 2013-12-11 | 东北石油大学 | Method for preparing nano-scale ZSM-5 molecular sieve by using coal ash |
| CN103787366A (en) * | 2014-01-26 | 2014-05-14 | 淮南师范学院 | Preparation method of low-cost ZSM-5 type zeolite molecular sieve, and application thereof |
| WO2017221192A1 (en) * | 2016-06-23 | 2017-12-28 | University Of The Western Cape | Process for production of high silica content zeolite from fly ash |
| CN106784917A (en) * | 2016-12-16 | 2017-05-31 | 哈尔滨工业大学深圳研究生院 | A kind of method of modifying of the PEM for all-vanadium flow battery |
| CN107697927A (en) * | 2017-11-14 | 2018-02-16 | 江苏理工学院 | A kind of preparation method using flyash as the NaA molecular sieve of raw material |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109621903A (en) * | 2019-01-31 | 2019-04-16 | 上海交通大学 | A method of preparing sludge base charcoal zeolite functional material |
| CN109824059A (en) * | 2019-03-13 | 2019-05-31 | 东北大学 | A kind of preparation method of ZSM-5 zeolite |
| CN109879295A (en) * | 2019-04-25 | 2019-06-14 | 太原理工大学 | A kind of ZSM-5 molecular sieve |
| CN110156044A (en) * | 2019-06-14 | 2019-08-23 | 河南理工大学 | A kind of preparation method of no sodium fly ash base ZSM-5 molecular sieve |
| CN111039301A (en) * | 2019-12-31 | 2020-04-21 | 青岛科技大学 | Method for preparing hierarchical pore ZSM-5 molecular sieve by using fly ash |
| CN111039301B (en) * | 2019-12-31 | 2022-03-08 | 青岛科技大学 | Method for preparing hierarchical pore ZSM-5 molecular sieve by using fly ash |
| CN114212799A (en) * | 2021-12-21 | 2022-03-22 | 黑龙江省能源环境研究院 | Coal ash pretreatment method for molecular sieve preparation |
| CN114212799B (en) * | 2021-12-21 | 2024-03-12 | 黑龙江省能源环境研究院 | Fly ash pretreatment method for molecular sieve preparation |
| CN114506856A (en) * | 2022-01-21 | 2022-05-17 | 贵州理工学院 | Method for preparing ZSM-5 molecular sieve from industrial silicon waste |
| CN115770609A (en) * | 2022-11-17 | 2023-03-10 | 华电电力科学研究院有限公司 | Preparation method of fly ash-based Fe/ZSM-5 mesoporous molecular sieve catalyst |
| CN115770609B (en) * | 2022-11-17 | 2024-04-19 | 华电电力科学研究院有限公司 | Preparation method of fly ash-based Fe/ZSM-5 mesoporous molecular sieve catalyst |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108892151A (en) | A kind of flyash ZSM-5 molecular sieve and preparation method thereof | |
| CN104291349B (en) | A kind of take flyash as the method that P type molecular sieve prepared by raw material | |
| CN101591023A (en) | A kind of method of utilizing aluminous fly-ash to prepare calcium silicate micro power | |
| CN112844447B (en) | Zeolite-based denitration catalyst and preparation method and application thereof | |
| CN102167338B (en) | Technology for preparing hydrated sodium aluminosilicate by utilizing high-alumina coal gangue and fly ash alkali soluble desiliconization | |
| CN102583410B (en) | Method for producing active calcium silicate by using fly ash desilication mother solution | |
| CN103103349B (en) | Method for decomposing bayan obo rare earth ore concentrate by acid and alkali combination at low temperature | |
| CN110354840A (en) | It is a kind of to prepare β-Bi2O3/BiVO4The new method of composite photocatalyst material | |
| CN106745027A (en) | A kind of flyash synthesizes the method for analcime | |
| CN106517237A (en) | Method for preparing NaY-type molecular sieve and ZSM-5 type molecular sieve by use of fly ash acid-process aluminum extraction residues and utilization method of fly ash | |
| CN102861566B (en) | Method for preparing bimetallic denitration catalyst by using coal ash | |
| CN107376957B (en) | Preparation method and application of red phosphorus-coated titanium dioxide nanofiber photocatalytic material | |
| CN106865586B (en) | A kind of method for preparing alumina type aeroge | |
| CN108059171A (en) | A kind of method of flyash synthesis HZSM-5 type zeolites | |
| CN103253681B (en) | Method for preparing Na-A/X or Na-A/X/P cocrystallized molecular sieve by lithium slag hydrothermal synthesis | |
| CN107758681B (en) | NaOH and Na2CO3Method for synthesizing 4A type molecular sieve by mixed alkali fusion fly ash | |
| CN103332711B (en) | Deep desilicication method of high-alumina fly ash | |
| CN103936045B (en) | A kind of method extracting aluminum oxide from flyash | |
| CN109336123A (en) | A method of using coal ash for manufacturing for soluble glass of high modulus | |
| CN108190926A (en) | A kind of preparation method of desiliconization flyash | |
| CN106865565A (en) | A kind of flyash synthesizes the method for X-type zeolite | |
| CN106044784A (en) | Method for producing high-purity silicon dioxide by utilizing flyash | |
| CN103014316A (en) | Novel method for processing lepidolite material | |
| CN105668597B (en) | The method of flyash soda acid combined extracting aluminium base product and silica-based products | |
| CN101172634A (en) | Technique for producing hydroted alumina and silicic acid with coal ash |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20181127 |
|
| RJ01 | Rejection of invention patent application after publication |