CN105600800A - Method for synthesizing CoAPO-41 molecular sieve - Google Patents

Method for synthesizing CoAPO-41 molecular sieve Download PDF

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CN105600800A
CN105600800A CN201610157962.7A CN201610157962A CN105600800A CN 105600800 A CN105600800 A CN 105600800A CN 201610157962 A CN201610157962 A CN 201610157962A CN 105600800 A CN105600800 A CN 105600800A
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molecular sieve
coapo
percentage composition
quality percentage
synthetic
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吴伟
张甜甜
魏小盟
白雪峰
肖林飞
张阳
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Heilongjiang University
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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
    • C01B37/00—Compounds having molecular sieve properties but not having base-exchange properties
    • C01B37/06—Aluminophosphates containing other elements, e.g. metals, boron
    • C01B37/065—Aluminophosphates containing other elements, e.g. metals, boron the other elements being metals only
    • 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
    • C01B39/54—Phosphates, e.g. APO or SAPO compounds
    • 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
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM

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Abstract

The invention discloses a method for synthesizing a CoAPO-41 molecular sieve and relates to a method for synthesizing a molecular sieve. The invention aims at solving the problems that relatively high acid site density cannot be formed without introducing a large quantity of Si atoms in the existing synthesis process of an SAPO-41 molecular sieve, but the Si atoms hardly enter the molecular sieve framework and are uniformly distributed on the framework to form a non-framework amorphous species which deposits in the pore orifices or pore channels of the molecular sieve to cause partial blocking of the pore orifices or pore channels. The method comprises the following steps: (I) preparing initial gel; and (II) crystallizing and roasting to obtain the CoAPO-41 molecular sieve. In the invention, the prepared CoAPO-41 molecular sieve is a spherical aggregate or crystal cluster consisting of nano rods, wherein the crystallizing time is only (1/2)-(1/3) of that of the prior art while mixed crystals are avoided; and the CoAPO-41 molecular sieve can be applied to the fields such as petrochemical industry as an environment-friendly acid catalyst.

Description

A kind of method of synthetic CoAPO-41 molecular sieve
Technical field
The present invention relates to the method for synthesis of molecular sieve.
Background technology
In existing SAPO-41 sieve synthesis procedure, must introduce a large amount of Si atoms and could form compared with peracidity bit density,But Si atom is difficult to enter framework of molecular sieve and on skeleton, is uniformly distributed and forms the unformed species of non-skeleton, thereby heavyAmass in the aperture place or duct of molecular sieve, cause the Partial Blocking in aperture or duct.
CoAPO-41 is skeleton P or P and the Al formation in Co part isomorphous substitution AlPO-41 aluminium phosphate molecular sieveThere is the molecular sieve of AFO topological structure, there is one dimension ellipse ten-ring duct.
AlPO-41 is by AlO4With PO4The aluminum phosphate molecule with AFO type topological structure of tetrahedron alternative arrangement compositionSieve, skeleton charge balance, does not have acidic site. Co atom is introduced to aluminium phosphate molecular sieve skeleton and replace P or P with partMake with Al the CoAPO-41 molecular sieve that the cobalt isomorphous replaces, can provide proton, tool with the hydrogen proton of skeleton negative electrical charge balanceThere is gentle acidity.
Summary of the invention
The present invention will solve and in existing SAPO-41 sieve synthesis procedure, must introduce a large amount of Si atoms and could form compared with peracidProperty bit density, but Si atom is difficult to enter framework of molecular sieve and on skeleton, is uniformly distributed and forms the amorphous article of non-skeletonKind, thereby be deposited in the aperture place or duct of molecular sieve, cause the problem of the Partial Blocking in aperture or duct, and provideA kind of method of synthetic CoAPO-41 molecular sieve.
A method for synthetic CoAPO-41 molecular sieve, specifically carry out according to following steps:
One, prepare initial gel: take quality percentage composition and be 85% phosphoric acid, secondary deionized water, boehmite,Di-n-butylamine and cobalt nitrate, the phosphoric acid that is first 85% by quality percentage composition mixes with secondary deionized water, obtainsReaction system under the stirring condition that is 800r/min～1000r/min, adds successively the thin water aluminium of plan at rotating speed in reaction systemStone, di-n-butylamine and cobalt nitrate, stir 20min～40min, obtains initial gel;
The phosphoric acid that described quality percentage composition is 85% and the mass ratio of secondary deionized water are 1:(3.5～4.5); Described matterThe phosphoric acid that amount percentage composition is 85% and the mass ratio of boehmite are 1:(0.5～0.7); Described quality percentage composition is85% phosphoric acid and the mass ratio of di-n-butylamine are 1:(1.5～2.0); Phosphoric acid and nitric acid that described quality percentage composition is 85%The mass ratio of cobalt is 1:(0.03～0.25);
Two, crystallization and roasting: initial gel is placed in to band teflon-lined stainless steel crystallizing kettle, in temperature isUnder the condition of 170 DEG C～190 DEG C, crystallization 8h～30h, is first cooled to 20 DEG C～25 DEG C by crystallization product, then at centrifugal rotational speedUnder condition for 4000r/min～6000r/min, centrifugation 10min～20min, then washing, in temperature isUnder the condition of 100 DEG C～120 DEG C, dry 12h～24h, is finally placed in Muffle furnace by dried crystallization product, in temperatureBe that under the condition of 500 DEG C～700 DEG C, roasting 8h～12h, makes CoAPO-41 molecular sieve.
The invention has the beneficial effects as follows: the SAPO-41 SAPO replacing with the silicon atom with identical topological structureMolecular sieve is compared, and adopts this method in AlPO-41 framework of molecular sieve, only to introduce a small amount of Co atom, preparationCoAPO-41 molecular sieve can produce abundant active sites, overcome in SAPO-41 sieve synthesis procedureCould form compared with peracidity bit density, Si atom because being difficult to enter framework of molecular sieve also because introducing a large amount of Si atomsOn skeleton, be uniformly distributed and form the unformed species of non-skeleton and be deposited in the aperture place or duct of molecular sieve,Cause the drawback such as Partial Blocking in aperture or duct, and consumption that can be by changing cobalt source in initial gel easilyThe acidity of CoAPO-41 molecular sieve is realized to meticulous modulation, there is the acidity of milder than SAPO-41.
It is the spherical poly-of nanometer rods composition that the present invention adopts pure phase CoAPO-41 molecular sieve prepared by the method for Co isomorphous substitutionCollective or druse; Crystallization time does not only have while introducing Co 1/2～1/3 of synthetic AlPO-41, and crystallization time significantly shortens.Because crystallite dimension reduces, can and acidic site density higher, will effectively improve product at molecule sieve aperture as catalystDiffusion in road, suppresses its carbon distribution inactivation, can be used as catalyst and is widely used in petrochemical industry production field.
CoAPO-41 supports the bifunctional catalyst with metal active center and acid site prepared by noble metal, at diesel oil andIn the processes such as the isomerization-visbreaking of lubricating oil, have broad application prospects. CoAPO-41 in the alkylated reaction of naphthalene and methyl alcoholMolecular sieve is expected to have suitable catalytic activity and the high selectivity to 2,6-DMN, and because acidity is gentleer, by toolThere is better carbon accumulation resisting ability.
The present invention is for a kind of method of synthetic CoAPO-41 molecular sieve.
Brief description of the drawings
Fig. 1 is the XRD spectra of the CoAPO-41/A molecular sieve prepared of embodiment mono-;
Fig. 2 is the SEM photo of the CoAPO-41/A molecular sieve prepared of embodiment mono-;
Fig. 3 is the XRD spectra of the CoAPO-41/B molecular sieve prepared of embodiment bis-;
Fig. 4 is the SEM photo of the CoAPO-41/B molecular sieve prepared of embodiment bis-;
Fig. 5 is the XRD spectra of the CoAPO-41/C molecular sieve prepared of embodiment tri-;
Fig. 6 is the SEM photo of the CoAPO-41/C molecular sieve prepared of embodiment tri-;
Fig. 7 is the XRD spectra of the CoAPO-41/D molecular sieve prepared of embodiment tetra-;
Fig. 8 is the SEM photo of the CoAPO-41/D molecular sieve prepared of embodiment tetra-.
Detailed description of the invention
Technical solution of the present invention is not limited to following cited detailed description of the invention, also comprises between each detailed description of the inventionAny combination.
Detailed description of the invention one: the method for a kind of synthetic CoAPO-41 molecular sieve described in present embodiment, specifically pressCarry out according to following steps:
One, prepare initial gel: take quality percentage composition and be 85% phosphoric acid, secondary deionized water, boehmite,Di-n-butylamine and cobalt nitrate, the phosphoric acid that is first 85% by quality percentage composition mixes with secondary deionized water, obtainsReaction system under the stirring condition that is 800r/min～1000r/min, adds successively the thin water aluminium of plan at rotating speed in reaction systemStone, di-n-butylamine and cobalt nitrate, stir 20min～40min, obtains initial gel;
The phosphoric acid that described quality percentage composition is 85% and the mass ratio of secondary deionized water are 1:(3.5～4.5); Described matterThe phosphoric acid that amount percentage composition is 85% and the mass ratio of boehmite are 1:(0.5～0.7); Described quality percentage composition is85% phosphoric acid and the mass ratio of di-n-butylamine are 1:(1.5～2.0); Phosphoric acid and nitric acid that described quality percentage composition is 85%The mass ratio of cobalt is 1:(0.03～0.25);
Two, crystallization and roasting: initial gel is placed in to band teflon-lined stainless steel crystallizing kettle, in temperature isUnder the condition of 170 DEG C～190 DEG C, crystallization 8h～30h, is first cooled to 20 DEG C～25 DEG C by crystallization product, then at centrifugal rotational speedUnder condition for 4000r/min～6000r/min, centrifugation 10min～20min, then washing, in temperature isUnder the condition of 100 DEG C～120 DEG C, dry 12h～24h, is finally placed in Muffle furnace by dried crystallization product, in temperatureBe that under the condition of 500 DEG C～700 DEG C, roasting 8h～12h, makes CoAPO-41 molecular sieve.
The beneficial effect of present embodiment is: the SAPO-41 silicon phosphate replacing with the silicon atom with identical topological structureAluminum molecular screen is compared, and adopts this method in AlPO-41 framework of molecular sieve, only to introduce a small amount of Co atom, systemStandby CoAPO-41 molecular sieve can produce abundant active sites, has overcome the sieve synthesis procedure at SAPO-41Middlely could form compared with peracidity bit density, Si atom because being difficult to enter framework of molecular sieve because introducing a large amount of Si atomsAnd on skeleton, be uniformly distributed and form the unformed species of non-skeleton and be deposited on aperture place or the duct of molecular sieveIn, cause the drawback such as Partial Blocking in aperture or duct, and can be by changing the consumption side in cobalt source in initial gelJust the acidity of CoAPO-41 molecular sieve is realized to meticulous modulation, there is the acidity of milder than SAPO-41.
It is the spherical poly-of nanometer rods composition that the present invention adopts pure phase CoAPO-41 molecular sieve prepared by the method for Co isomorphous substitutionCollective or druse; Crystallization time does not only have while introducing Co 1/2～1/3 of synthetic AlPO-41, and crystallization time significantly shortens.Because crystallite dimension reduces, can and acidic site density higher, will effectively improve product at molecule sieve aperture as catalystDiffusion in road, suppresses its carbon distribution inactivation, can be used as catalyst and is widely used in petrochemical industry production field.
CoAPO-41 supports the bifunctional catalyst with metal active center and acid site prepared by noble metal, at diesel oil andIn the processes such as the isomerization-visbreaking of lubricating oil, have broad application prospects. CoAPO-41 in the alkylated reaction of naphthalene and methyl alcoholMolecular sieve is expected to have suitable catalytic activity and the high selectivity to 2,6-DMN, and because acidity is gentleer, by toolThere is better anti-carbon energy.
Detailed description of the invention two: present embodiment is different from detailed description of the invention one: the plan described in step 1Al in boehmite2O3Quality percentage composition be 71.3%; The quality percentage composition of the cobalt nitrate described in step 1 is99%; The quality percentage composition of the di-n-butylamine described in step 1 is 99%. Other is identical with detailed description of the invention one.
Detailed description of the invention three: present embodiment is different from one of detailed description of the invention one or two: in step 2Be under the condition of 170 DEG C～190 DEG C in temperature, crystallization 12h～24h. Other is identical with detailed description of the invention one or two.
Detailed description of the invention four: present embodiment is different from one of detailed description of the invention one to three: in step 1The phosphoric acid that described quality percentage composition is 85% and the mass ratio of cobalt nitrate are 1:(0.06～0.08). Other and specific embodiment partyFormula one to three is identical.
Detailed description of the invention five: present embodiment is different from one of detailed description of the invention one to four: in step 1The phosphoric acid that described quality percentage composition is 85% and the mass ratio of cobalt nitrate are 1:(0.12～0.14). Other and specific embodiment partyFormula one to four is identical.
Detailed description of the invention six: present embodiment is different from one of detailed description of the invention one to five: in step 1The phosphoric acid that described quality percentage composition is 85% and the mass ratio of cobalt nitrate are 1:(0.18～0.2). Other and specific embodiment partyFormula one to five is identical.
Detailed description of the invention seven: present embodiment is different from one of detailed description of the invention one to six: in step 2Be under the condition of 185 DEG C in temperature, crystallization 24h. Other is identical with detailed description of the invention one to six.
Detailed description of the invention eight: present embodiment is different from one of detailed description of the invention one to seven: in step 2Under the condition that is 4000r/min at centrifugal rotational speed again, centrifugation 15min. Other is identical with detailed description of the invention one to seven.
Detailed description of the invention nine: present embodiment is different from one of detailed description of the invention one to eight: in step 2Be under the condition of 110 DEG C in temperature, dry 12h. Other is identical with detailed description of the invention one to eight.
Detailed description of the invention ten: present embodiment is different from one of detailed description of the invention one to nine: in step 2Be under the condition of 540 DEG C in temperature, roasting 10h. Other is identical with detailed description of the invention one to nine.
Adopt following examples to verify beneficial effect of the present invention:
Embodiment mono-:
The method of a kind of synthetic CoAPO-41 molecular sieve described in the present embodiment, specifically carry out according to following steps:
One, prepare initial gel: take phosphoric acid that 4.52g quality percentage composition is 85%, 18.72g secondary deionized water,2.8g boehmite, 8g di-n-butylamine and 0.18g cobalt nitrate, the phosphoric acid that is first 85% by quality percentage composition and twoInferior deionized water mixes, and obtains reaction system, under the stirring condition that is 850r/min at rotating speed, in reaction systemAdd successively boehmite, di-n-butylamine and cobalt nitrate, stir 20min, obtain initial gel;
Two, crystallization and roasting: initial gel is placed in to band teflon-lined stainless steel crystallizing kettle, in temperature isUnder the condition of 185 DEG C, crystallization 24h, is first cooled to 20 DEG C～25 DEG C by crystallization product, then is 4000r/min at centrifugal rotational speedCondition under, centrifugation 20min, then washing, is under the condition of 110 DEG C in temperature, dry 12h, finally will doCrystallization product after dry is placed in Muffle furnace, is that under the condition of 540 DEG C, roasting 10h, makes CoAPO-41 and divide in temperatureSon sieve;
Al in boehmite described in step 12O3Quality percentage composition be 71.3%; Nitre described in step 1The quality percentage composition of acid cobalt is 99%; The quality percentage composition of the di-n-butylamine described in step 1 is 99%.
Fig. 1 is the XRD spectra of the CoAPO-41/A molecular sieve prepared of embodiment mono-, as can be seen from Figure 1, and at 2 θAngle is 20.64 °, 20.15 °, 21.26 °, locates all to have the characteristic diffraction peak of AFO topological structure, says for 22.20 ° and 22.25 °Bright without other stray crystal;
Fig. 2 is the SEM photo of the CoAPO-41/A molecular sieve prepared of embodiment mono-, as can be seen from Figure 2, and this sampleIt is the druse that nanometer rods forms.
Embodiment bis-:
The method of a kind of synthetic CoAPO-41 molecular sieve described in the present embodiment, specifically carry out according to following steps:
One, prepare initial gel: take phosphoric acid that 4.52g quality percentage composition is 85%, 18.72g secondary deionized water,2.8g boehmite, 8g di-n-butylamine and 0.35g cobalt nitrate, the phosphoric acid that is first 85% by quality percentage composition and twoInferior deionized water mixes, and obtains reaction system, under the stirring condition that is 800r/min at rotating speed, in reaction systemAdd successively boehmite, di-n-butylamine and cobalt nitrate, stir 20min, obtain initial gel;
Two, crystallization and roasting: initial gel is placed in to band teflon-lined stainless steel crystallizing kettle, in temperature isUnder the condition of 185 DEG C, crystallization 24h, is first cooled to 20 DEG C～25 DEG C by crystallization product, then is 4000r/min at centrifugal rotational speedCondition under, centrifugation 20min, then washing, is under the condition of 110 DEG C in temperature, dry 12h, finally will doCrystallization product after dry is placed in Muffle furnace, is that under the condition of 540 DEG C, roasting 10h, makes CoAPO-41 and divide in temperatureSon sieve;
Al in boehmite described in step 12O3Quality percentage composition be 71.3%; Nitre described in step 1The quality percentage composition of acid cobalt is 99%; The quality percentage composition of the di-n-butylamine described in step 1 is 99%.
Fig. 3 is the XRD spectra of the CoAPO-41/B molecular sieve prepared of embodiment bis-, as can be seen from Figure 3, and at 2 θAngle is 20.64 °, 20.15 °, 21.26 °, locates all to have the characteristic diffraction peak of AFO topological structure, says for 22.20 ° and 22.25 °Bright without other stray crystal;
Fig. 4 is the SEM photo of the CoAPO-41/B molecular sieve prepared of embodiment bis-, as can be seen from Figure 4, and this sampleIt is the druse being formed by nanometer rods.
Embodiment tri-:
The method of a kind of synthetic CoAPO-41 molecular sieve described in the present embodiment, specifically carry out according to following steps:
One, prepare initial gel: take phosphoric acid that 4.52g quality percentage composition is 85%, 18.72g secondary deionized water,2.8g boehmite, 8g di-n-butylamine and 0.59g cobalt nitrate, the phosphoric acid that is first 85% by quality percentage composition and twoInferior deionized water mixes, and obtains reaction system, under the stirring condition that is 800r/min at rotating speed, in reaction systemAdd successively boehmite, di-n-butylamine and cobalt nitrate, stir 20min, obtain initial gel;
Two, crystallization and roasting: initial gel is placed in to band teflon-lined stainless steel crystallizing kettle, in temperature isUnder the condition of 185 DEG C, crystallization 24h, is first cooled to 20 DEG C～25 DEG C by crystallization product, then is 4000r/min at centrifugal rotational speedCondition under, centrifugation 20min, then washing, is under the condition of 110 DEG C in temperature, dry 12h, finally will doCrystallization product after dry is placed in Muffle furnace, is that under the condition of 540 DEG C, roasting 10h, makes CoAPO-41 and divide in temperatureSon sieve;
Al in boehmite described in step 12O3Quality percentage composition be 71.3%; Nitre described in step 1The quality percentage composition of acid cobalt is 99%; The quality percentage composition of the di-n-butylamine described in step 1 is 99%.
Fig. 5 is the XRD spectra of the CoAPO-41/C molecular sieve prepared of embodiment tri-, as can be seen from Figure 1, and at 2 θBe 20.64 °, 20.15 °, 21.26 °, locate all to have the characteristic diffraction peak of AFO topological structure, explanation for 22.20 ° and 22.25 °Without other stray crystal;
Fig. 6 is the SEM photo of the CoAPO-41/C molecular sieve prepared of embodiment tri-, as can be seen from Figure 6, and this sampleIt is the sphere aggregates being formed by nanometer rods.
Embodiment tetra-:
The method of a kind of synthetic CoAPO-41 molecular sieve described in the present embodiment, specifically carry out according to following steps:
One, prepare initial gel: take phosphoric acid that 4.52g quality percentage composition is 85%, 18.72g secondary deionized water,2.8g boehmite, 8g di-n-butylamine and 0.88g cobalt nitrate, the phosphoric acid that is first 85% by quality percentage composition and twoInferior deionized water mixes, and obtains reaction system, under the stirring condition that is 800r/min at rotating speed, in reaction systemAdd successively boehmite, di-n-butylamine and cobalt nitrate, stir 20min, obtain initial gel;
Two, crystallization and roasting: initial gel is placed in to band teflon-lined stainless steel crystallizing kettle, in temperature isUnder the condition of 185 DEG C, crystallization 24h, is first cooled to 20 DEG C～25 DEG C by crystallization product, then is 4000r/min at centrifugal rotational speedCondition under, centrifugation 15min, then washing, is under the condition of 110 DEG C in temperature, dry 12h, finally will doCrystallization product after dry is placed in Muffle furnace, is that under the condition of 540 DEG C, roasting 10h, makes CoAPO-41 and divide in temperatureSon sieve;
Al in boehmite described in step 12O3Quality percentage composition be 71.3%; Nitre described in step 1The quality percentage composition of acid cobalt is 99%; The quality percentage composition of the di-n-butylamine described in step 1 is 99%.
Fig. 7 is the XRD spectra of the CoAPO-41/D molecular sieve prepared of embodiment tetra-, as can be seen from Figure 7, and at 2 θBe 20.64 °, 20.15 °, 21.26 °, locate all to have the characteristic diffraction peak of AFO topological structure, explanation for 22.20 ° and 22.25 °Without other stray crystal;
Fig. 8 is the SEM photo of the CoAPO-41/D molecular sieve prepared of embodiment tetra-, as can be seen from Figure 8, and this sampleIt is the sphere aggregates that nanometer rods forms.

Claims (10)

1. a method for synthetic CoAPO-41 molecular sieve, is characterized in that a kind of side of synthetic CoAPO-41 molecular sieveMethod is carried out according to following steps:
One, prepare initial gel: take quality percentage composition and be 85% phosphoric acid, secondary deionized water, boehmite,Di-n-butylamine and cobalt nitrate, the phosphoric acid that is first 85% by quality percentage composition mixes with secondary deionized water, obtains anti-Answer system, under the stirring condition that is 800r/min～1000r/min at rotating speed, to add successively in reaction system boehmite,Di-n-butylamine and cobalt nitrate, stir 20min～40min, obtains initial gel;
The phosphoric acid that described quality percentage composition is 85% and the mass ratio of secondary deionized water are 1:(3.5～4.5); Described matterThe phosphoric acid that amount percentage composition is 85% and the mass ratio of boehmite are 1:(0.5～0.7); Described quality percentage composition is 85%Phosphoric acid and the mass ratio of di-n-butylamine be 1:(1.5～2.0); The phosphoric acid that described quality percentage composition is 85% and cobalt nitrateMass ratio is 1:(0.03～0.25);
Two, crystallization and roasting: initial gel is placed in to band teflon-lined stainless steel crystallizing kettle, is 170 in temperatureDEG C～condition of 190 DEG C under, crystallization 8h～30h, is first cooled to 20 DEG C～25 DEG C by crystallization product, then at centrifugal rotational speed isUnder the condition of 4000r/min～6000r/min, centrifugation 10min～20min, then washing, is 100 DEG C～120 DEG C in temperatureCondition under, dry 12h～24h, is finally placed in Muffle furnace by dried crystallization product, is 500 DEG C～700 DEG C in temperatureCondition under, roasting 8h～12h, makes CoAPO-41 molecular sieve.
2. the method for a kind of synthetic CoAPO-41 molecular sieve according to claim 1, is characterized in that step 1Described in boehmite in Al2O3Quality percentage composition be 71.3%; The quality hundred of the cobalt nitrate described in step 1Dividing content is 99%; The quality percentage composition of the di-n-butylamine described in step 1 is 99%.
3. the method for a kind of synthetic CoAPO-41 molecular sieve according to claim 1, is characterized in that step 2In under temperature is the condition of 170 DEG C～190 DEG C, crystallization 12h～24h.
4. the method for a kind of synthetic CoAPO-41 molecular sieve according to claim 1, is characterized in that step 1Described in the quality percentage composition phosphoric acid that is 85% and the mass ratio of cobalt nitrate be 1:(0.06～0.08).
5. the method for a kind of synthetic CoAPO-41 molecular sieve according to claim 1, is characterized in that step 1Described in the quality percentage composition phosphoric acid that is 85% and the mass ratio of cobalt nitrate be 1:(0.12～0.14).
6. the method for a kind of synthetic CoAPO-41 molecular sieve according to claim 1, is characterized in that step 1Described in the quality percentage composition phosphoric acid that is 85% and the mass ratio of cobalt nitrate be 1:(0.18～0.2).
7. the method for a kind of synthetic CoAPO-41 molecular sieve according to claim 1, is characterized in that step 2In under temperature is the condition of 185 DEG C, crystallization 24h.
8. the method for a kind of synthetic CoAPO-41 molecular sieve according to claim 1, is characterized in that step 2In under the condition that is 4000r/min at centrifugal rotational speed again, centrifugation 15min.
9. the method for a kind of synthetic CoAPO-41 molecular sieve according to claim 1, is characterized in that step 2In under temperature is the condition of 110 DEG C, dry 12h.
10. the method for a kind of synthetic CoAPO-41 molecular sieve according to claim 1, is characterized in that step 2In under temperature is the condition of 540 DEG C, roasting 10h.
CN201610157962.7A 2016-03-18 2016-03-18 Method for synthesizing CoAPO-41 molecular sieve Pending CN105600800A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112624137A (en) * 2019-09-24 2021-04-09 中国石油化工股份有限公司 AFN structure molecular sieve composed of cobalt, phosphorus and aluminum, and synthetic method and application thereof

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