CN110510627A - The preparation method of P type zeolite molecular sieve and resulting P type zeolite molecular sieve - Google Patents
The preparation method of P type zeolite molecular sieve and resulting P type zeolite molecular sieve Download PDFInfo
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- CN110510627A CN110510627A CN201910892749.4A CN201910892749A CN110510627A CN 110510627 A CN110510627 A CN 110510627A CN 201910892749 A CN201910892749 A CN 201910892749A CN 110510627 A CN110510627 A CN 110510627A
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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
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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
- C01B39/46—Other types characterised by their X-ray diffraction pattern and their defined composition
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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
- C01B39/50—Zeolites wherein inorganic bases or salts occlude channels in the lattice framework, e.g. sodalite, cancrinite, nosean, hauynite
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
- C01P2006/65—Chroma (C*)
Abstract
The present invention provides a kind of preparation methods of P type zeolite molecular sieve, using residue of aluminum-extracted pulverized fuel ash as starting material, are calcined to obtain calcined fine coal powder residue of aluminum-extracted first, obtain then in turn through ageing, Crystallizing treatment.The present invention also provides a kind of P type zeolite molecular sieves, with excellent whiteness and absorption property.Preparation method of the invention has carried out reasonable and effective recycling and reusing to residue of aluminum-extracted pulverized fuel ash, alleviate environmental pressure, P type zeolite molecular sieve obtained is functional, preparation method simple process of the invention, easy to operate, the high production efficiency of safety, without using excessive reagent, at low cost and environmental pollution is small, is suitable for plant-scale production.
Description
Technical field
The present invention relates to molecular sieve manufacturing fields, and in particular to the preparation method of a kind of P type zeolite molecular sieve and made
The P type zeolite molecular sieve obtained.
Background technique
Molecular sieve is a kind of alumino-silicate compound with cubic lattice, is mainly made up of silicon, aluminium oxygen bridge connection
Spacious skeleton structure has the uniform duct in many apertures and the very big hole of marshalling, internal surface area, furthermore in the structure
Water also lower containing electricity price and ionic radius biggish metal ion and compound state.Since hydrone constantly escapes after heating,
But crystal framework structure is constant, thus forms the identical cavity of many sizes, and there are many identical micropore phases of diameter again for cavity
Even, the small material molecule of channel diameter is adsorbed on cavity inside, and obtains molecule exclusion bigger than duct, to make difference
The molecule of size shape separates, and plays the role of sieving molecule, thus is referred to as molecular sieve.
Traditional industrial zeolite molecular sieve synthesis is usually using sodium metasilicate, silica as silicon source, aluminium hydroxide, meta-aluminic acid
Sodium is as silicon source, using oxygen sodium oxide molybdena, oxygen potassium oxide etc. as alkali source, higher cost.The comprehensive utilization of flyash is in recent years
Research hotspot, the existing technology that p-zeolite is prepared using flyash as raw material, can mainly divide according to the difference of synthesis step at present
It is two kinds: hydrothermal synthesis method and alkali fusion hydrothermal synthesis method.Chinese patent ZL 201210506177.X is disclosed is with flyash
The method that raw material prepares single Zeolite mineral species P type zeolite successively mixes flyash through hydrochloric acid and sodium hydroxide and potassium hydroxide
After alkaline solution treatment, then with silica flour, NaOH and distilled water match resulting mixture in proportion, is placed in micro-wave oven and heats, so
It is placed in autoclave, after ripening and crystallization, obtains single Zeolite mineral species P type zeolite molecular sieve.China
Patent ZL 201310045511.0 discloses the method using industrial solid wastes synthesis P type zeolite molecular sieve, by solid waste
Be made into mixed liquor with the aqueous solution of alkali, heating stirring is reacted, then add silicon source or silicon source adjustment silica alumina ratio reacted, Gu
It is washed with water after liquid separation, CaCl is added2Or FeC12Solution, drying-granulating obtain P type zeolite molecular sieve.
It is carried out as raw material mentioning in the way of aluminium processing is a kind of high-value-use by flyash, such as by " a step acid extracting " from powder
Aluminium oxide is extracted in coal ash, the residue after mentioning aluminium mainly contains silica and alumina composition, can be to ring without processing discharge
Border causes seriously to pollute, and offal treatment then consumes huge economic cost.Therefore, it is badly in need of exploitation new technique to flyash
Residue of aluminum-extracted carries out recycling and reusing, to reduce the harm to environment, and improves the utilization rate of resource.
Summary of the invention
In order to overcome aforementioned drawback existing in the prior art, it is an object of the present invention to provide a kind of P type zeolites point
The preparation method of son sieve, can efficiently use residue of aluminum-extracted pulverized fuel ash, prepare the P type zeolite molecular sieve of high quality.
It is a further object of the present invention to provide a kind of P type zeolite molecular sieves.
The preparation method of P type zeolite molecular sieve provided by the invention using residue of aluminum-extracted pulverized fuel ash as starting material, by with
Lower step is made:
S1: the residue of aluminum-extracted pulverized fuel ash is calcined 2~6 hours at 500~800 DEG C, calcined fine coal powder is obtained and mentions aluminium
Residue;And
S2: calcined fine coal powder residue of aluminum-extracted made from step S1 is mixed with alkali source solution, is carried out at 40~70 DEG C old
Change, then heats to 80~95 DEG C of progress crystallization, separating obtained product is simultaneously drying to obtain.
Preparation method of the invention first calcines to carry out carbonization treatment residue of aluminum-extracted pulverized fuel ash, contains in residue of aluminum-extracted
More free carbon, if specific aim is not removed, resulting molecular sieve whiteness is bad, and absorption property is also affected.Decarburization
Treated, and material is sufficiently mixed dissolution with alkali source solution again, obtains final P type zeolite molecular sieve by ageing, crystallization, inhales
Attached to have excellent performance, calcium ion-exchanged amount can reach 300mg/g or more, be much larger than 4A molecular sieve national standard (280mg/g), whiteness
It can be used in the special dimensions such as washing assisant 95% or more.
In some embodiments, the residue of aluminum-extracted pulverized fuel ash is flyash after " a step acid extracting " extracts aluminium oxide
Resulting residue.
In some embodiments, in the residue of aluminum-extracted pulverized fuel ash by mass percentage include 15~20% Al2O3With
And 50~60% SiO2。
In some embodiments, the alkali source solution is the sodium hydroxide or potassium hydroxide aqueous solution of 2~5mol/L,
Amount ratio with the calcined fine coal powder residue of aluminum-extracted is 100:15~30 (mL/g), i.e., the alkali source solution pair of every 100mL
Calcined fine coal powder residue of aluminum-extracted described in 15~30g should be used.
In some embodiments, during the ageing, mixing speed is 600~1000 revs/min, digestion time
It is 2~6 hours, suitably increasing mixing speed in ageing process can make residue of aluminum-extracted and alkali source solution better contact with dissolution.
In some embodiments, during the crystallization, mixing speed is 200~500 revs/min, crystallization time
It is 10~36 hours, mixing speed is suitably reduced in crystallization process can be conducive to the growth of crystal.
In some embodiments, the drying is 2~6 hours dry at 80~100 DEG C.
The present invention also provides a kind of P type zeolite molecular sieves, by the described in any item preparation methods of above technical scheme
It is made.
In some embodiments, whiteness >=95% of the P type zeolite molecular sieve.
In some embodiments, the calcium ion-exchanged amount of the P type zeolite molecular sieve is 300~325mg/g.
The preparation method of P type zeolite molecular sieve provided by the invention has the advantage that
(1) preparation method of the present invention has carried out reasonable and effective recycling and reusing to residue of aluminum-extracted pulverized fuel ash, alleviates
Environmental pressure, low cost product obtained, functional, economic value with higher.
(2) P type zeolite molecular sieve absorption property made from preparation method of the present invention is excellent, and calcium ion-exchanged amount is high, also has
There is good whiteness, expand molecular sieve uses field, in addition, p-zeolite produced by the present invention is also with higher pure
Degree and good microscopic appearance.
(3) preparation method simple process of the invention, easy to operate, the high production efficiency of safety, without using excessive reagent,
At low cost and environmental pollution is small, is suitable for plant-scale production.
Detailed description of the invention
Fig. 1 is X-ray powder diffraction (XRD) figure for the residue of aluminum-extracted pulverized fuel ash that embodiment uses.
Fig. 2 is scanning electron microscope (SEM) figure for the residue of aluminum-extracted pulverized fuel ash that embodiment uses.
Fig. 3 is the calcined XRD diagram of residue of aluminum-extracted pulverized fuel ash that embodiment uses.
Fig. 4 is the XRD diagram of p-zeolite made from embodiment 2.
Fig. 5 is the SEM figure of p-zeolite made from embodiment 2.
Specific embodiment
Below in conjunction with specific embodiment, further details of the technical solution of the present invention.
In an embodiment of the present invention, used starting material is residue of aluminum-extracted pulverized fuel ash, can be provided from Shenhua standard
Source comprehensive exploitation Co., Ltd aluminium oxide pilot plant, in main ingredient, Al2O3Mass percentage be 18.09%, SiO2
Mass percentage be 52.40%, Fe2O3Mass percentage be 0.42%, TiO2Mass percentage be
4.33%.Characterization result is shown in Fig. 1, Fig. 2.
In an embodiment of the present invention, the test of calcium ion-exchanged amount is carried out according to QB/T 1768-2003 method, whiteness
Test is carried out according to 13176.1 method of GB/T.
In an embodiment of the present invention, unless otherwise instructed, used reagent or material are commercial product, are used
Device or operating method be this field common apparatus or operating method.
1 residue of aluminum-extracted pulverized fuel ash of embodiment prepares P type zeolite molecular sieve
Include the following steps:
1) by residue of aluminum-extracted pulverized fuel ash in 500 DEG C of calcinings, 6 hours obtained calcined fine coal powder residue of aluminum-extracted;
2) 20g calcined fine coal powder residue of aluminum-extracted is weighed, the NaOH aqueous solution 100mL of 4mol/L is measured, is uniformly mixed, in water
At 40 DEG C of bath, adjustment revolving speed is 800 revs/min of strong stirring 5h, then is warming up to 95 DEG C, and adjustment revolving speed is 400 revs/min of middling speeds
Stir 10h;By the solid product filtering in solution, filter cake filters again after distill water washing, again filter cake obtained by filtering in
100 DEG C drying 2 hours, powdered P type zeolite molecular sieve is made.
After tested, the p-zeolite whiteness that prepared by embodiment 1 is 95%, and calcium ion-exchanged amount is 300mg/g.
2 residue of aluminum-extracted pulverized fuel ash of embodiment prepares P type zeolite molecular sieve
Include the following steps:
1) residue of aluminum-extracted pulverized fuel ash is in 700 DEG C of calcinings, 3 hours obtained calcined fine coal powder residue of aluminum-extracted, XRD diagram such as Fig. 3 institute
Show, is compared with Fig. 1 it is found that mutually substantially unchanged with calcined object before calcination by residue of aluminum-extracted pulverized fuel ash;
2) 15g calcined fine coal powder residue of aluminum-extracted is weighed, the NaOH aqueous solution 100mL of 2mol/L is measured, is uniformly mixed, in water
At 60 DEG C of bath, adjustment revolving speed is 1000 revs/min of strong stirring 4h, then is warming up to 90 DEG C, and adjustment revolving speed is in 500 revs/min
Speed stirring 16h;By the solid product filtering in solution, filter cake filters again after distilling water washing, again filtering gained filter cake
It is 3 hours dry in 95 DEG C, powdered P type zeolite molecular sieve is made.
The XRD diagram of p-zeolite prepared by embodiment 2 is as shown in figure 4, SEM schemes as shown in figure 5, Fig. 4 shows the P of preparation
Type molecular sieve purity is higher, and Fig. 5 shows that the p-zeolite sample particle of preparation is uniform in size, and microscopic appearance is preferable.
After tested, the p-zeolite whiteness that prepared by embodiment 2 is 96%, and calcium ion-exchanged amount is 325mg/g.
3 residue of aluminum-extracted pulverized fuel ash of embodiment prepares P type zeolite molecular sieve
Include the following steps:
1) residue of aluminum-extracted pulverized fuel ash is in 800 DEG C of calcinings, 2 hours obtained calcined fine coal powder residue of aluminum-extracted;
2) 25g calcined fine coal powder residue of aluminum-extracted is weighed, the NaOH aqueous solution 100mL of 5mol/L is measured, is uniformly mixed, in water
At 70 DEG C of bath, adjustment revolving speed is 600 revs/min of strong stirring 6h, then is warming up to 80 DEG C, and adjustment revolving speed is 200 revs/min of middling speeds
Stir 36h;By the solid product filtering in solution, filter cake filters again after distill water washing, again filter cake obtained by filtering in
80 DEG C drying 6 hours, powdered P type zeolite molecular sieve is made.
After tested, the p-zeolite whiteness that prepared by embodiment 3 is 97%, and calcium ion-exchanged amount is 315mg/g.
4 residue of aluminum-extracted pulverized fuel ash of embodiment prepares P type zeolite molecular sieve
Include the following steps:
1) 600 DEG C of residue of aluminum-extracted pulverized fuel ash calcinings, 4 hours obtained calcined fine coal powder residue of aluminum-extracted;
2) 30g calcined fine coal powder residue of aluminum-extracted is weighed, the NaOH aqueous solution 100mL of 3mol/L is measured, is uniformly mixed, in water
At 50 DEG C of bath, adjustment revolving speed is 700 revs/min of strong stirring 5h, then is warming up to 85 DEG C, and adjustment revolving speed is 300 revs/min of middling speeds
Stirring is for 24 hours;By the solid product filtering in solution, filter cake filters again after distill water washing, again filter cake obtained by filtering in
90 DEG C drying 5 hours, powdered P type zeolite molecular sieve is made.
After tested, the p-zeolite whiteness that prepared by embodiment 4 is 96%, and calcium ion-exchanged amount is 310mg/g.
Comparative example
Whiteness is tested to p-zeolite made from Chinese patent application CN 108658092A, is lower than 90%.
Industrial applicibility
P type zeolite molecular sieve absorption property produced by the present invention is excellent it can be seen from embodiment 1-4 and comparative example, calcium
Ion exchange capacity has good whiteness up to 300~325mg/g, can reach 95% or more, can be used for washing and help
The industries such as agent.Preparation process simple process of the invention, easy to operate, the high production efficiency of safety, at low cost and environmental pollution is small,
It is very suitable to industrialized production.
Unless limited otherwise, term used herein is the normally understood meaning of those skilled in the art.
Embodiment described in the invention is merely for exemplary purpose, the protection scope being not intended to limit the invention,
Those skilled in the art can be made within the scope of the invention various other replacements, changes and improvements, thus, the present invention is not limited to
Above embodiment, and be only defined by the claims.
Claims (10)
1. a kind of preparation method of P type zeolite molecular sieve, which is characterized in that using residue of aluminum-extracted pulverized fuel ash as starting material, pass through
Following steps are made:
S1: the residue of aluminum-extracted pulverized fuel ash is calcined 2~6 hours at 500~800 DEG C, obtains calcined fine coal powder residue of aluminum-extracted;
And
S2: calcined fine coal powder residue of aluminum-extracted made from step S1 is mixed with alkali source solution, is aged at 40~70 DEG C, so
After be warming up to 80~95 DEG C of progress crystallization, separating obtained product is simultaneously drying to obtain.
2. preparation method according to claim 1, which is characterized in that the residue of aluminum-extracted pulverized fuel ash is that flyash passes through " one
Walk acid extracting " extract resulting residue after aluminium oxide.
3. preparation method according to claim 2, which is characterized in that in the residue of aluminum-extracted pulverized fuel ash by mass percentage
Include 15~20% Al2O3And 50~60% SiO2。
4. preparation method according to claim 1-3, which is characterized in that the alkali source solution is 2~5mol/L
Sodium hydroxide or potassium hydroxide aqueous solution, be 100:15~30 (mL/ with the amount ratio of the calcined fine coal powder residue of aluminum-extracted
g)。
5. preparation method according to claim 1-4, which is characterized in that during the ageing, stirring speed
Degree is 600~1000 revs/min, and digestion time is 2~6 hours.
6. preparation method according to claim 1-5, which is characterized in that during the crystallization, stirring speed
Degree is 200~500 revs/min, and crystallization time is 10~36 hours.
7. preparation method according to claim 1-6, which is characterized in that the drying is dry at 80~100 DEG C
Dry 2~6 hours.
8. a kind of P type zeolite molecular sieve, which is characterized in that be made by the described in any item preparation methods of claim 1-7.
9. P type zeolite molecular sieve according to claim 8, which is characterized in that the whiteness of the P type zeolite molecular sieve >=
95%.
10. P type zeolite molecular sieve according to claim 8 or claim 9, which is characterized in that the calcium of the P type zeolite molecular sieve from
Sub- exchange capacity is 300~325mg/g.
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Cited By (1)
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CN112978758A (en) * | 2021-04-09 | 2021-06-18 | 陕西科技大学 | Method for preparing Na-P type zeolite by utilizing natural clinoptilolite |
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