CN108408735A - A method of preparing SUZ-4 molecular sieves using silicon ash - Google Patents
A method of preparing SUZ-4 molecular sieves using silicon ash Download PDFInfo
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- CN108408735A CN108408735A CN201810485232.9A CN201810485232A CN108408735A CN 108408735 A CN108408735 A CN 108408735A CN 201810485232 A CN201810485232 A CN 201810485232A CN 108408735 A CN108408735 A CN 108408735A
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- 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
- C01B39/04—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 using at least one organic template directing agent, e.g. an ionic quaternary ammonium compound or an aminated compound
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- 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
Abstract
A method of 4 molecular sieves of SUZ being prepared using silicon ash, belong to the preparing technical field of molecular sieve, can solve the problems, such as that the synthesis cost of 4 molecular sieves of existing SUZ is high and complicated using waste synthesis of molecular sieve process.Preparation method is as follows：Silicon ash is directly mixed in a certain ratio with 4 crystal seeds of SUZ, potassium hydroxide and deionized water, gained mixture is put into hydrothermal reaction kettle, crystallization 0.5 4 days at 100 200 DEG C filter the sample after crystallization, washing can obtain 4 molecular sieve solid powder of SUZ after dry.The method and process of involved synthesis 4 molecular sieves of SUZ is simple, easy in the present invention, not only greatly reduces the synthesis cost of the molecular sieve, also achieves the higher value application of silicon ash.
Description
Technical field
The invention belongs to the preparing technical fields of molecular sieve, and in particular to a kind of to prepare SUZ-4 molecular sieves using silicon ash
Method.
Background technology
SUZ-4 is a kind of micropore Si-Al molecular sieve.Its unique pore passage structure, a large amount of B acid position make the molecular sieve select
The every field for selecting absorption, separation and catalysis has good actual application prospect.Compared with other molecular sieves, SUZ-4 points
The preparation process of son sieve is complicated, time consumption and energy consumption.To solve this problem, patent CN102241407A report it is a kind of utilize crystal seed
Glue synthesizes the preparation method of SUZ-4 molecular sieves.The program realizes SUZ-4 molecular sieves low temperature, quickly synthesis.However, mesh
The primary raw material of preceding SUZ-4 Zeolite synthesis is still the silicon salt and aluminium salt of chemical raw material, and higher synthesis cost limits this
The commercial Application of molecular sieve.Therefore, a kind of new process being prepared SUZ-4 molecular sieves using waste of exploitation is particularly important.
Silicon ash, also known as SILICA FUME are the ferroalloy industries in smelting duriron or industrial silicon when the high temperature in ore-smelting electric furnace
（2600 DEG C or more）The silica and silicon gas of generation after contacting with the air rapid oxidation condensation and formed a kind of ultra-fine nothing
Shape powder, is to smelt silicon systems product tail gas by-product.This substance is in addition to containing a large amount of SiO2（Account for 85% or more）Outside, also contain
There is a certain amount of Al2O3.After being contacted with water, silicon ash dissolves exhaust quickly, assembles, is agglomerating, forms amorphous silicon alumina gel.To sum up,
We have reason to believe that silicon ash will be expected to the silicon salt and aluminium salt of substitution chemical raw material, become the cheap of synthesis SUZ-4 molecular sieves
Silicon and aluminum source.
2011, king University of Science and Technology of Thailand Worathanakul et al. synthesized SUZ- using bagasse ash as common silicon source
4 molecular sieves.They are the study found that only when the input amount ratio of bagasse ash and Ludox is less than 50:When 50, can just it obtain pure
SUZ-4 molecular sieves.With the increase of bagasse ash input amount, it is miscellaneous to occur other molecular sieves such as MER, PHI and Linde in system
Phase.When using bagasse ash as silicon source completely, then it can not synthesize SUZ-4 molecular sieves.2013, Jaroonvechatam etc.
People synthesizes SUZ-4 molecular sieves using rice husk ash as common silicon source.It is much like with the studies above that they study discovery, that is, works as paddy
The ratio of shell ash can get the SUZ-4 molecular sieves of high-purity at 50%, and the ratio regular meeting for increasing rice husk ash causes the life of MER dephasigns
At.This is the research report for relating to the use of waste synthesis SUZ-4 molecular sieves so far.In addition, about use waste as
Material synthesis molecular sieve with reduce manufacturing cost technical solution have patent report, as patent CN1O3787354A,
CN103435064A etc. using plant residue-flyash as Material synthesis molecular sieve, for another example patent CN1334142,
CN105645433A etc. is using natural mineral-kaolin as Material synthesis molecular sieve.However, these existing technical solutions are all
Raw material need to be pre-processed（Such as soda acid processing, high-temperature process）Crystallization is carried out again after obtaining required substance.These skills
Although art scheme reduces synthesis cost, but increase synthesis procedure, keeps synthesis more cumbersome.Therefore, such method is at present simultaneously
Industrialized production is not implemented.
Invention content
The present invention is directed to the preparation method synthesis cost height of existing SUZ-4 molecular sieves and utilizes waste synthesis of molecular sieve
Process complexity problem, a kind of method preparing SUZ-4 molecular sieves using silicon ash is provided.
The present invention adopts the following technical scheme that：
A method of SUZ-4 molecular sieves being prepared using silicon ash, are included the following steps：
The first step prepares SUZ-4 crystal seeds, including crystal seed glue or seed particles, 0.2g aluminium flakes is dissolved in by 1.92g KOH and 10g
In the KOH aqueous solutions of deionized water composition, above-mentioned solution and 15.68g are contained into 30% SiO2Ludox, 5.68g contain 25% four
The tetraethyl ammonium hydroxide aqueous solution of ethyl ammonium hydroxide and the mixing of 7.98 g deionized waters, form white gels, and stirring half is small
The gel of formation is transferred in the water heating kettle of 100 ml by Shi Hou, under the rotating speed of 20rpm, in 150 DEG C of dynamic crystallizations 4 days, is obtained
To the SUZ-4 crystal seed glue of 41g；Or above-mentioned crystal seed glue is obtained to the solid SUZ-4 crystal seeds of 3.5g after being filtered, washed, drying, be calcined
Particle；
Second step, synthesize SUZ-4 molecular sieves, synthesized using SUZ-4 crystal seeds, by silicon ash, SUZ-4 crystal seeds, potassium hydroxide and go from
It after sub- water proportionally mixes, is placed in water heating kettle, under 100-200 DEG C of crystallization temperature, crystallization 0.5-4d can be obtained knot
The SUZ-4 molecular sieves that brilliant degree is 100%, wherein SiO in silicon ash2Content be 85%, silicon ash is with SiO2Meter；SiO2∶KOH∶H2O's
Molar ratio is：21.2~31.6: 7.9~12.5: 139.4~998；The additive amount of crystal seed is 10% or more gained crystal seed total amount.
Synthesis of molecular sieve described in second step can not use SUZ-4 crystal seeds yet and synthesize, it is water-soluble that silicon source is dissolved in potassium hydroxide
After in liquid, silicon ash is added, after stirring half an hour, adds template aqueous solution, continues after stirring half an hour, it is solidifying to form white
The white gels are transferred in water heating kettle by glue, under the rotating speed of 20rpm, under 180 DEG C of crystallization temperature, and crystallization 2d
Obtain the SUZ-4 molecular sieves that crystallinity is 100%, wherein silicon source is with Al2O3It counts, SiO in silicon ash2Content be 85%, silicon ash with
SiO2Meter, template are containing 25% tetraethyl ammonium hydroxide, SiO2：KOH：Al2O3：TEAOH：H2The molar ratio of O is 21.2:
7.9:0.5:2.6:498.6。
Crystal seed described in second step can also be the SUZ-4 molecular sieves synthesized by the step, and additive amount is to close
At 10% or more of gained molecular sieve total amount.
Crystallization described in second step is dynamic crystallization or static crystallization.
Beneficial effects of the present invention are as follows：
1. the present invention under the conditions of having existing for crystal seed, is not necessarily to additional silicon and aluminum source, the SiO contained in silicon ash is fully utilized2And
Al2O3, pure SUZ-4 molecular sieves can be synthesized under certain hydrothermal condition.In addition, with the objects such as flyash, kaolin are utilized
The technology path of matter synthesis of molecular sieve is compared, the SiO in silicon ash2And Al2O3With very high " activity ", therefore, business is purchased next
Silicon ash can be directly thrown into synthetic system carry out SUZ-4 molecular sieves synthesis, without to silicon ash carry out any activation or
Preprocessing means.
It is used in follow-up synthesis 2. the SUZ-4 molecular sieves of gained of the invention are alternatively arranged as crystal seed.
3. the present invention without using crystal seed when synthesizing, the additive amount of silicon source is only silicon source additive amount in conventional synthesis process
Half.
It is also the recycling of silicon ash 4. the proposition of present invention process not only greatly reduces SUZ-4 Zeolite synthesis costs
Using a new way is provided, reach the unification of economic benefit and environmental benefit.
Description of the drawings
Fig. 1 is the XRD spectra of SUZ-4 molecular sieves prepared by the present invention；
Fig. 2 is the XRD spectra of 2 amorphous substance of comparative example.
Specific implementation mode
Embodiment 1
The first step prepares SUZ-4 crystal seeds, including crystal seed glue or seed particles
0.2g aluminium flakes are dissolved in the KOH aqueous solutions being made of 1.92g KOH and 10g deionized waters, by above-mentioned solution with
15.68g containing 30% SiO2Ludox, 5.68g containing 25% tetraethyl ammonium hydroxide tetraethyl ammonium hydroxide aqueous solution and
7.98 g deionized waters mix, and form white gels, and after stirring half an hour, the gel of formation is transferred to the water heating kettle of 100 ml
It is interior, under the rotating speed of 20 rpm, in 150 DEG C of dynamic crystallizations 4 days, obtain the SUZ-4 crystal seed glue of 41g；Or above-mentioned crystal seed glue is passed through
Be filtered, washed, dry, be calcined after 3.5 g solid SUZ-4 seed particles；
Second step is synthesized SUZ-4 molecular sieves, is synthesized using SUZ-4 crystal seeds
5.2 g silicon ashes are added in the KOH aqueous solutions formed by the KOH and 33.3 g deionized waters of 1.92 g, are acutely being stirred
In the case of mixing, 4.1 g of SUZ-4 crystal seeds glue is added, is further continued for stirring half an hour.The total material of formation is transferred to 100 ml
In water heating kettle, under the rotating speed of 20 rpm, in 150 DEG C of dynamic crystallizations 4 days, obtained SUZ-4 molecular sieves were free of stray crystal, crystallization
Degree is 100%.Its XRD spectra is shown in Fig. 1.
Embodiment 2
The additive amount of deionized water is reduced to 9.3g, 200 DEG C of dynamic crystallization 12h, remaining condition repeats embodiment 1, can be tied
The SUZ-4 molecular sieves that brilliant degree is 100%.
Embodiment 3
The amount of KOH is changed to 2.5 g, and added crystal seed glue is changed to the SUZ-4 seed particles of 0.4 g, in 180 DEG C of static crystallizations 4
It, remaining condition repeats embodiment 1, and the SUZ-4 molecular sieves that crystallinity is 100% can be obtained.
Embodiment 4
The amount of silicon ash is changed to 7.8 g, the amount of KOH is changed to 3 g, and deionized water addition is changed to 66.6 g, added crystal seed glue
It is changed to 7g.In 100 DEG C of dynamic crystallizations 2 days, remaining condition repeated embodiment 1, and the SUZ-4 molecules that crystallinity is 100% can be obtained
Sieve.
Embodiment 5
The amount of silicon ash is changed to 6.1 g, added crystal seed is 1.2 g of SUZ-4 molecular sieves of the synthesis gained of embodiment 1, in 150 DEG C
Dynamic crystallization 1 day, remaining condition repeat embodiment 1, and the SUZ-4 molecular sieves that crystallinity is 100% can be obtained.
Embodiment 6
0.1 g aluminium flakes are dissolved in the KOH aqueous solutions formed by the KOH and 29.0 g deionized waters of 1.92 g, by 5.2 g silicon ashes
It will enter into above-mentioned solution.After stirring half an hour, 5.68 g tetraethyl ammonium hydroxide aqueous solutions are added（Containing 25% tetraethyl
Ammonium hydroxide）, continue to stir half an hour.By the white gels of formation（Mole group becomes：21.2SiO2: 7.9KOH:
0.5Al2O3: 2.6 TEAOH: 498.6H2O）It is transferred in the rotatable water heating kettles of 100 ml, under the rotating speed of 20 rpm, in
180 DEG C of dynamic crystallizations 2 days obtain the pure SUZ-4 molecular sieves that crystallinity is 100%.
Comparative example 1
The aluminium flake of 0.2g is dissolved in the KOH aqueous solutions formed by 1.92gKOH and 10g deionized waters；By 15.68g Ludox
（Containing 30% SiO2）, the tetraethyl ammonium hydroxide aqueous solution of 5.68g（Containing 25% TEAOH）And 7.98 g deionized waters formed
Mixed solution is added with vigorous stirring in above-mentioned clear solution, after white gels to be formed, is further continued for stirring half an hour.By shape
At gel（Mole group becomes：21.2SiO2: 7.9KOH: 1.0Al2O3: 2.6 TEAOH: 498.6H2O）It is transferred to 100
In the rotatable water heating kettles of ml, under the rotating speed of 20 rpm, after 150 DEG C of dynamic crystallizations 4 days, it is 100% to obtain crystallinity
SUZ-4 molecular sieves.
Comparative example 2
Example 1 is repeated, but is added without SUZ-4 crystal seeds, products therefrom is amorphous substance after crystallization.
Comparative example 3
Example 6 is repeated, but is added without silicon source, products therefrom is amorphous substance after crystallization.
Claims (4)
1. a kind of method preparing SUZ-4 molecular sieves using silicon ash, it is characterised in that：Include the following steps：
The first step prepares SUZ-4 crystal seeds, including crystal seed glue or seed particles：0.2g aluminium flakes are dissolved in by 1.92g KOH and 10g
In the KOH aqueous solutions of deionized water composition, above-mentioned solution and 15.68g are contained into 30% SiO2Ludox, 5.68g contain 25% four
The tetraethyl ammonium hydroxide aqueous solution of ethyl ammonium hydroxide and the mixing of 7.98 g deionized waters, form white gels, and stirring half is small
The gel of formation is transferred in the water heating kettle of 100ml by Shi Hou, under the rotating speed of 20 rpm, in 150 DEG C of dynamic crystallizations 4 days, is obtained
To the SUZ-4 crystal seed glue of 41g；Or above-mentioned crystal seed glue is obtained to the solid SUZ-4 crystal seeds of 3.5g after being filtered, washed, drying, be calcined
Particle；
Second step is synthesized SUZ-4 molecular sieves, is synthesized using SUZ-4 crystal seeds：By silicon ash, SUZ-4 crystal seeds, potassium hydroxide and go from
It after sub- water proportionally mixes, is placed in water heating kettle, under 100-200 DEG C of crystallization temperature, crystallization 0.5-4d can be obtained knot
The SUZ-4 molecular sieves that brilliant degree is 100%, wherein SiO in silicon ash2Content be 85%, silicon ash is with SiO2Meter；SiO2∶KOH∶H2O's
Molar ratio is：21.2~31.6: 7.9~12.5: 139.4~998；The additive amount of crystal seed is 10% or more gained crystal seed total amount.
2. a kind of method preparing SUZ-4 molecular sieves using silicon ash according to claim 1, it is characterised in that：Second step
Described in synthesis of molecular sieve, also can not use SUZ-4 crystal seeds synthesize, after silicon source is dissolved in potassium hydroxide aqueous solution, add
Silicon ash adds template aqueous solution after stirring half an hour, continues after stirring half an hour, forms white gels, and the white is solidifying
Glue is transferred in water heating kettle, and under the rotating speed of 20rpm, under 180 DEG C of crystallization temperature, crystallization 2d can be obtained crystallinity and be
100% SUZ-4 molecular sieves, wherein silicon source is with Al2O3It counts, SiO in silicon ash2Content be 85%, silicon ash is with SiO2Meter, template
For containing 25% tetraethyl ammonium hydroxide, SiO2：KOH：Al2O3：TEAOH：H2The molar ratio of O is 21.2:7.9:0.5:2.6:
498.6。
3. a kind of method preparing SUZ-4 molecular sieves using silicon ash according to claim 1, it is characterised in that：Second step
Described in crystal seed can also be the SUZ-4 molecular sieves that are synthesized by the step, additive amount is synthesis gained molecular sieve
10% or more of total amount.
4. a kind of method preparing SUZ-4 molecular sieves using silicon ash according to claim 1, it is characterised in that：The crystalline substance
Turn to dynamic crystallization or static crystallization.
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Cited By (5)
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| CN109626393A (en) * | 2019-02-26 | 2019-04-16 | 中触媒新材料股份有限公司 | A kind of preparation method for the SUZ-4 that hedgehog is spherical |
| CN109704364A (en) * | 2019-02-21 | 2019-05-03 | 太原理工大学 | A kind of synthetic method of regulation SUZ-4 Molecular Sieve Morphology |
| CN112723378A (en) * | 2019-10-28 | 2021-04-30 | 中国石油化工股份有限公司 | Method for synthesizing SUZ-4 molecular sieve |
| CN112723369A (en) * | 2019-10-28 | 2021-04-30 | 中国石油化工股份有限公司 | Preparation method of SUZ-4 molecular sieve |
| CN113617330A (en) * | 2021-09-18 | 2021-11-09 | 太原理工大学 | Low-cost and fast Pb adsorption device2+Preparation method of Na-SUZ-4 molecular sieve |
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| CN113617330A (en) * | 2021-09-18 | 2021-11-09 | 太原理工大学 | Low-cost and fast Pb adsorption device2+Preparation method of Na-SUZ-4 molecular sieve |
| CN113617330B (en) * | 2021-09-18 | 2023-04-11 | 太原理工大学 | Low-cost and fast Pb adsorption device 2+ Preparation method of Na-SUZ-4 molecular sieve |
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