CN104649294B - Method for improving relative crystallinity of synthetic NaY zeolite - Google Patents
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Abstract
The invention provides a method for improving the relative crystallinity of synthetic NaY zeolite. The method mainly includes: in a directing agent preparation process, mixing a silicon source, an aluminum source and an oxygen-containing organic matter, and conducting ageing at 15DEG C-60DEG C for 1-60h to prepare a directing agent; in a gel preparation process, mixing the silicon source, the directing agent and an alkaline solution, performing stirring at 10-90DEG C for 1-80h, and then adding the aluminum source. The method provided by the invention can synthesize NaY zeolite with crystallinity of more than 90% and a SiO2/Al2O3 molar ratio of 5.0-5.5 within 10h-40h, and can increase the relative crystallinity of the synthetic molecular sieve product by over 5% without changing the existing NaY production equipment in current industry, thus being of great significance to improvement of the molecular sieve production economic benefits.
Description
Technical field
The present invention relates to a kind of method of the relative crystallinity of nay zeolite improving synthesis, belong to inorganic material and catalysis
Agent preparing technical field.
Background technology
Y zeolite, because acid, the good heat of its flourishing 3 D pore canal, adjustable change and hydrothermal stability widely should
For oil refining industry.Degree of crystallinity and silica alumina ratio (sio2/al2o3) it is the topmost influence factor of y type zeolite nature and function
One of.The higher sample of relative crystallinity has higher heat stability and hydrothermal stability.When being applied to catalytic cracking, relatively
High crystallization reservation degree means more active center, higher catalytic performance；Improve the relative crystallization of initial synthetic sample
Degree can improve the crystallization reservation degree of sample after reaction, increases the economic benefit of product.
China nay zeolite Year's consumption is about 50,000 tons about, and nay zeolite Year's consumption in the whole world is about ten thousand tons of 50-70,
It is molecular sieve catalytic material the most large.Nay zeolite is as the primary raw material producing super steady y zeolite (usy molecular sieve), its property
The performance of usy molecular sieve can be directly affected, and then affect the performance of catalyst.The raising of nay zeolite properties, can not only
Improve the stability in catalytic cracking catalyst active component usy process of producing molecular sieve, improve the operating flexibility producing, with
When also will improve usy molecular sieve degree of crystallinity, to improve catalyst performance and expand catalyst business competitiveness have weight
Want meaning.
At present the method for industrial production nay molecular sieve mostly using grace company of the similar U.S. in us3639099 and
Directing agent method proposed in us3671191, the method can synthesize in 28 hours degree of crystallinity more than 83%, sial exists
5.0 about nay zeolite product, but its degree of crystallinity to reach more than 90% relatively difficult.Further, since the sial of synthetic sample
Compare relatively low it is impossible to bear last handling process complexity exacting terms, in processing procedure, crystallinity loss is greatly it is difficult to meet high
The requirement of performance Catalyst Production.In recent years, catalytic cracking catalyst technology of preparing makes rapid progress, and comprises a series of among these
The appearance of nay technology for modifying, it is also proposed higher requirement to the performance of nay zeolite, commercial production is in the urgent need to further
Improve the sial when degree of crystallinity of nay product.
Therefore develop the synthesis that a kind of raising that is effective, being suitable for industrialized production synthesizes nay zeolite relative crystallinity
Method, is still one of this area problem to be solved.
Content of the invention
It is an object of the invention to provide a kind of effective, phase of the nay zeolite improving synthesis that is being suitable for industrialized production
Method to degree of crystallinity, to improve the relative crystallinity of the nay zeolite of synthesis at short notice.
For reaching above-mentioned purpose, the invention provides a kind of method of the relative crystallinity of nay zeolite improving synthesis, the party
Method mainly includes step:
(1) directed agents are prepared: silicon source, silicon source and oxygen-bearing organic matter are pressed mol ratio (1.2 × 10-2～1.5 × 102) contain
Oxygen organic: (10～30) na2o:al2o3: (10～30) sio2: (150～450) h2O mixes, by mixture at 15 DEG C～60 DEG C
Lower ageing 1～60h, prepares directed agents；
(2) prepare gel reaction mixture: at 10 DEG C～90 DEG C, it is directed to agent and alkaline solution is added in silicon source,
Stirring 1～80h, adds silicon source, stirs, prepared gel reaction mixture；Wherein, control the proportioning of gel reaction mixture
For (1～4) na2o:al2o3: (6～10) sio2: (100～300) h2O, and wherein directed agents consumption accounts for reactant mixture weight hundred
Divide the 1%～60% of ratio；
(3) the gel reaction mixture of preparation is warming up to 80～120 DEG C of crystallization 10～70h, then through filtering, washing,
Drying steps are obtained nay zeolite product.
According to specific embodiments of the present invention, in the method for the relative crystallinity of the nay zeolite of above-mentioned raising synthesis,
Described silicon source is selected from one of Ludox, waterglass, white carbon, sodium silicate, positive silicic acid or multiple, preferably water glass
Glass；Source of aluminium is selected from one or more of sodium metaaluminate, aluminum sulfate, aluminum nitrate or boehmite, preferably partially
Sodium aluminate etc..
According to specific embodiments of the present invention, in the method for the relative crystallinity of the nay zeolite of above-mentioned raising synthesis,
Preferably, in the step of described preparation directed agents, oxygen-bearing organic matter is oxolane, ethanol or acetone.
According to specific embodiments of the present invention, in the method for the relative crystallinity of the nay zeolite of above-mentioned raising synthesis,
It is by after silicon source, silicon source mixing in step (1), be blended into oxygen-bearing organic matter and water, stirring and evenly mixing must mix at 15 DEG C～60 DEG C
Compound.
According to specific embodiments of the present invention, in the method for the relative crystallinity of the nay zeolite of above-mentioned raising synthesis,
Preferably, in described step (2) (step preparing gel reaction mixture), it is directed to agent and alkaline solution is added in silicon source
Stir 1h～50h afterwards.
According to specific embodiments of the present invention, in the method for the relative crystallinity of the nay zeolite of above-mentioned raising synthesis,
Preferably, it is to prepare gel reaction mixture at 10 DEG C～70 DEG C in step (2).
According to specific embodiments of the present invention, in the method for the relative crystallinity of the nay zeolite of above-mentioned raising synthesis,
Alkaline solution described in step (2) is sodium hydroxide solution, ammonia, sodium bicarbonate solution, in sodium aluminate solution a kind of or
Multiple.
According to specific embodiments of the present invention, in the method for the relative crystallinity of the nay zeolite of above-mentioned raising synthesis,
Silicon source described in step (2) is selected from one of Ludox, waterglass, white carbon, sodium silicate, positive silicic acid or multiple, described
Silicon source is selected from one or more of sodium metaaluminate, aluminum sulfate, aluminum nitrate or boehmite.
According to specific embodiments of the present invention, in the method for the relative crystallinity of the nay zeolite of above-mentioned raising synthesis,
Preferably, in step (2), directed agents consumption accounts for the 1%～20% of described gel reaction mixture weight.
In the method for the relative crystallinity of nay zeolite of raising synthesis provided by the present invention, mainly will be oxygen-containing organic
Thing is added in directed agents so that the activity of directed agents increases；And using being directed to agent and alkaline solution adds under agitation
Enter in silicon source, so that directed agents is better dispersed in silicon source, then add silicon source, can be by the phase of the nay zeolite of synthesis
More than 5 percentage points are improved to degree of crystallinity.Additionally, in the synthetic method of the present invention, the ageing time of directed agents and gel
The crystallization time of reactant mixture is all relatively short so as to power consumption reduces.The method of the present invention can synthesize in 10h～40h
Degree of crystallinity more than 90%, sio2/al2o3Mol ratio is 5.0～5.5 nay zeolite.
In the method for the relative crystallinity of nay zeolite improving synthesis of the present invention, the step not referred in detail is for example brilliant
The filtration of change product, washing, drying and other steps can be carried out according to the routine operation of art.In the present invention, crystallization product is excellent
Choosing is to be dried at 60 DEG C～160 DEG C.
Present invention also offers the nay zeolite preparing according to methods described, its degree of crystallinity more than 90%, sio2/al2o3
Mol ratio is 5.0～5.5.
In sum, the synthetic method of the high silica alumina ratio nay zeolite of the present invention has the advantage that
(1) under conditions of low alkalinity relatively, the low silica alumina ratio that feeds intake, in the short period of time can be by the phase of sinteticses
5 percentage points are improved to degree of crystallinity, and the silica alumina ratio of product does not decline；
(2) do not change existing industry nay process units, be not required to increase miscellaneous equipment, you can carry out industrialized production.
Brief description
Fig. 1 is the xrd figure of the nay molecular sieve that embodiment 1 prepares.
Fig. 2 is the xrd figure of the nay molecular sieve that embodiment 2 prepares.
Fig. 3 is the xrd figure of the nay molecular sieve that embodiment 3 prepares.
Fig. 4 is the xrd figure of the nay molecular sieve that embodiment 4 prepares.
Fig. 5 is the xrd figure of the nay molecular sieve that embodiment 5 prepares.
Fig. 6 is the xrd figure of the nay molecular sieve that embodiment 6 prepares.
Fig. 7 is the xrd figure of the nay molecular sieve that embodiment 7 prepares.
Fig. 8 is the xrd figure of the nay molecular sieve that comparative example 1 prepares.
Fig. 9 is the xrd figure of the nay molecular sieve that comparative example 2 prepares.
Specific embodiment
Describe the enforcement of technical solution of the present invention in detail below by way of specific embodiment and had the advantage that, but not
Can regard as to the present invention can practical range any restriction.
In each embodiment and comparative example, the relative crystallinity of nay zeolite synthesizing and the mensure of silica alumina ratio adopt
Bruker d8 advance(Germany bruker) type x-ray diffraction instrument, experiment condition is: cuka radiation (0.1541nm), pipe electricity
Pressure 40kv, tube current 40ma.The mensure of relative crystallinity is that (" standard of chemical industry converges according to sh/t 0340-92 standard method
Compile ", China Standards Press, publish within 2000) carry out.The mensure of silica alumina ratio is according to sh/t 0339-92 standard method
(" standard of chemical industry compilation ", China Standards Press publish for 2000) are carried out, and calculate the crystalline substance of nay zeolite according to formula (1)
After born of the same parents' constant, calculate by breck-flanigen formula: si/al=(25.858- α)/(α -24.191).
Wherein,
α lattice constant,
λ-cuk α1Radiation wavelength
h2+k2+l2- x-ray diffraction Miller index quadratic sum.
It is 040617 that the zeolite standard specimen as degree of crystallinity standard used in embodiment and comparative example comes from numbering
Industrial nay reference, records the sio of this zeolite with x optical diffraction method2/al2o3For 5.1, and its degree of crystallinity is set as 100%.
Embodiment 1
The present embodiment provides a kind of method of the relative crystallinity of nay zeolite improving synthesis, and it comprises the following steps:
Take 75g waterglass (sio2Content is 28.45wt%, na2O content is 8.89wt%), add 75g high alkali deflection aluminium acid sodium
(na2O content is 21.11wt%, al2o3Content is 3.16wt%), 34.09g oxolane (analysis pure) and 30g water mix homogeneously
Stir 1h, aging 16h at 33 DEG C afterwards, make directed agents；
Take 200g waterglass (sio2Content is 28.45wt%, na2O content is 8.89wt%), put into and be placed in 60 DEG C of water-baths
Beaker in, under conditions of stirring, sequentially add the above-mentioned directed agents of 26.81g, 68.52g high alkali deflection aluminium acid sodium (na2O content is
21.11wt%, al2o3Content is 3.16wt%) and 50g water, add 129.83g aluminum sulfate (al after stirring 1h2o3Content is
7.60wt%) stir, prepared gel reaction mixture；
By above-mentioned gel reaction mixture load reactor at 96 DEG C crystallization 40h, then filter, washing is dried to obtain
Nay zeolite.
The nay molecular sieve of gained is characterized with xrd technology, the xrd figure obtaining is as shown in figure 1, record above-mentioned nay boiling
The silica alumina ratio of stone is 5.32, and degree of crystallinity is 96%.
Embodiment 2
The present embodiment provides a kind of method of the nay zeolite relative crystallinity improving synthesis, and it comprises the following steps:
Take 80g waterglass (sio2Content is 28.45wt%, na2O content is 8.89wt%), add 40g high alkali deflection aluminium acid sodium
(na2O content is 21.11wt%, al2o3Content is 3.16wt%), after 3.45g oxolane (analysis pure) and 20g water mix homogeneously
Stir 1h, aging 6h at 51 DEG C, make directed agents；
In the preparation process of gel reaction mixture, the consumption of each raw material and charging sequence are constant, simply in directed agents, height
After alkali sodium aluminate solution is added sequentially in waterglass, stirs 8h, then add aluminum sulfate, after stirring, be obtained solidifying
Glue reactant mixture；
Above-mentioned gel reaction mixture is loaded reactor crystallization 28h at 96 DEG C, then filters, washing is dried to obtain
Nay zeolite.
The nay molecular sieve of gained is characterized with xrd technology, the xrd figure obtaining is as shown in Fig. 2 record above-mentioned nay boiling
The silica alumina ratio of stone is 5.21, and degree of crystallinity is 94%.
Embodiment 3
The present embodiment provides a kind of method of the nay zeolite relative crystallinity improving synthesis, and it comprises the following steps:
Take 80g waterglass (sio2Content is 28.45wt%, na2O content is 8.89wt%), add 40g high alkali deflection aluminium acid sodium
(na2O content is 21.11wt%, al2o3Content is 3.16wt%), after 34.09g ethanol (analysis pure) and 20g water mix homogeneously
Stir 1h, aging 6h at 21 DEG C, make directed agents；
In the preparation process of gel reaction mixture, the consumption of each raw material is constant, simply in directed agents, high alkali deflection aluminium acid sodium
After solution is added sequentially in waterglass, stirs 48h, then add aluminum sulfate, after stirring, prepared gel reaction mixing
Thing；
Above-mentioned gel reaction mixture is loaded reactor crystallization 11h at 96 DEG C, then filters, washing is dried to obtain
Nay zeolite.
The nay molecular sieve of gained is characterized with xrd technology, the xrd figure obtaining is as shown in figure 3, record above-mentioned nay boiling
The silica alumina ratio of stone is 5.16, and degree of crystallinity is 95%.
Embodiment 4
The present embodiment provides a kind of method of the nay zeolite relative crystallinity improving synthesis, and it comprises the following steps:
Take 75g waterglass (sio2Content is 28.45wt%, na2O content is 8.89wt%), add 75g high alkali deflection aluminium acid sodium
(na2O content is 21.11wt%, al2o3Content is 3.16wt%), after 3.45g ethanol (analysis pure) and 30g water mix homogeneously 21
Stir 1h, aging 16h at DEG C, make directed agents；
Take 255g waterglass (sio2Content is 28.45wt%, na2O content is 8.89wt%), add in 60 DEG C of stirred in water bath
Enter the above-mentioned directed agents of 50g, 110.53g high alkali deflection aluminium acid sodium (na2O content is 21.11wt%, al2o3Content is 3.16wt%), stir
After mixing 8h, add 135g aluminum sulfate (al2o3Content is 7.60wt%) and 300g water stir after, prepared gel reaction is mixed
Compound；
By above-mentioned gel reaction mixture load reactor at 96 DEG C crystallization 24h, then filter, washing is dried to obtain
Nay zeolite.
The nay molecular sieve of gained is characterized with xrd technology, the xrd figure obtaining is as shown in figure 4, record above-mentioned nay boiling
The silica alumina ratio of stone is 5.33, and degree of crystallinity is 94%.
Embodiment 5
The present embodiment provides a kind of method of the relative crystallinity of nay zeolite improving synthesis, and it comprises the following steps:
Take 80g waterglass (sio2Content is 28.45wt%, na2O content is 8.89wt%), add 40g high alkali deflection aluminium acid sodium
(na2O content is 21.11wt%, al2o3Content is 3.16wt%), after 34.09g acetone (analysis pure) and 20g water mix homogeneously
Stir 1h, aging 16h at 51 DEG C, make directed agents；
Take 100g waterglass (sio2Content is 28.45wt%, na2O content is 8.89wt%), add in 60 DEG C of stirred in water bath
Enter the above-mentioned directed agents of 50g, 40g high alkali deflection aluminium acid sodium (na2O content is 21.11wt%, al2o3Content is 3.16wt%), stir 36h
Afterwards, add 115g aluminum sulfate (al2o3Content is 7.60wt%) and 100g water stir after, prepared gel reaction mixes
Thing；
By above-mentioned gel reaction mixture load reactor at 96 DEG C crystallization 36h, then filter, washing is dried to obtain
Nay zeolite.
The nay molecular sieve of gained is characterized with xrd technology, the xrd figure obtaining is as shown in figure 5, record above-mentioned nay boiling
The silica alumina ratio of stone is 5.28, and degree of crystallinity is 95%.
Embodiment 6
The present embodiment provides a kind of method of the relative crystallinity of nay zeolite improving synthesis, and it comprises the following steps:
Take 75g waterglass (sio2Content is 28.45wt%, na2O content is 8.89wt%), add 75g high alkali deflection aluminium acid sodium
(na2O content is 21.11wt%, al2o3Content is 3.16wt%), after 3.45g acetone (analysis pure) and 30g water mix homogeneously 21
Stir 1h, aging 16h at DEG C, make directed agents；
Take 255g waterglass (sio2Content is 28.45wt%, na2O content is 8.89wt%), add in 60 DEG C of stirred in water bath
Enter the above-mentioned directed agents of 50g, 110.53g high alkali deflection aluminium acid sodium (na2O content is 21.11wt%, al2o3Content is 3.16wt%), stir
After mixing 36h, add 135g aluminum sulfate (al2o3Content be 7.60wt%) and 300g water stir after, prepared gel reaction
Mixture；By above-mentioned gel reaction mixture load reactor at 96 DEG C crystallization 18h, then filter, washing is dried to obtain
Nay zeolite.
The nay molecular sieve of gained is characterized with xrd technology, the xrd figure obtaining is as shown in fig. 6, record above-mentioned nay boiling
The silica alumina ratio of stone is 5.40, and degree of crystallinity is 93%.
Embodiment 7
The present embodiment provides a kind of method of the relative crystallinity of nay zeolite improving synthesis, and it comprises the following steps:
Take 75g waterglass (sio2Content is 28.45wt%, na2O content is 8.89wt%), add 75g high alkali deflection aluminium acid sodium
(na2O content is 21.11wt%, al2o3Content is 3.16wt%) and 34.09g ethanol (analyze pure) mix homogeneously after at 33 DEG C
Aging 16h, makes directed agents；
Take 100g waterglass (sio2Content is 28.45wt%, na2O content is 8.89wt%), add in 60 DEG C of stirred in water bath
Enter the above-mentioned directed agents of 70g, 45g high alkali deflection aluminium acid sodium (na2O content is 21.11wt%, al2o3Content is 3.16wt%), stir 36h
Afterwards, add 155g aluminum sulfate (al2o3Content is 7.60wt%) and 100g water stir after, prepared gel reaction mixes
Thing；By above-mentioned gel reaction mixture load reactor at 96 DEG C crystallization 18h, then filter, washing be dried to obtain nay boiling
Stone.
The nay molecular sieve of gained is characterized with xrd technology, the xrd figure obtaining is as shown in fig. 7, record above-mentioned nay boiling
The silica alumina ratio of stone is 5.40, and degree of crystallinity is 93%.
Comparative example 1
This comparative example provides a kind of method of synthesis nay zeolite, and it comprises the following steps:
Take 75g waterglass (sio2Content is 28.45wt%, na2O content is 8.89wt%), add 75g high alkali deflection aluminium acid sodium
(na2O content is 21.11wt%, al2o3Content is 3.16wt%) after mix homogeneously at 33 DEG C aging 16h, make directed agents；
The consumption of the preparation process of gel reaction mixture and wherein each raw material is with embodiment 1；
Above-mentioned gel reaction mixture is loaded reactor crystallization 40h at 96 DEG C, then filters, washing is dried to obtain
Nay zeolite.
The nay molecular sieve of gained is characterized with xrd technology, the xrd figure obtaining is as shown in figure 8, record above-mentioned nay boiling
The silica alumina ratio of stone is 5.15, and degree of crystallinity is 89%.
Comparative example 2
This comparative example provides a kind of method of synthesis nay zeolite, and it comprises the following steps:
The preparation method of directed agents and the various raw materials being adopted and consumption are all with comparative example 1；
The preparation of gel reaction mixture is substantially same as Example 4 with the various raw materials being adopted and consumption.This contrast
Prepare the difference of gel reaction mixture in example and embodiment 4 to be: under stirring condition in 60 DEG C of water bath with thermostatic control, general
Waterglass, directed agents, aluminum sulfate solution are added sequentially in high alkali deflection aluminium acid sodium solution, after stirring, prepared gel reaction
Mixture.And, it is that above-mentioned gel reaction mixture is loaded reactor crystallization 60h at 96 DEG C, then mistake in this comparative example
Filter, washing is dried to obtain nay zeolite.
The nay molecular sieve of gained is characterized with xrd technology, the xrd figure obtaining is as shown in figure 9, record above-mentioned nay boiling
The silica alumina ratio of stone is 5.40, and degree of crystallinity is 85%.
Claims (9)
1. a kind of method of the relative crystallinity of nay zeolite improving synthesis, the method comprising the steps of:
(1) directed agents are prepared: silicon source, silicon source and oxygen-bearing organic matter are pressed mol ratio (1.2 × 10-2～1.5 × 102) oxygen-containing have
Machine thing: (10～30) na2o:al2o3: (10～30) sio2: (150～450) h2O mixes, and mixture is old at 15 DEG C～60 DEG C
Change 1～60h, prepare directed agents；Wherein, described oxygen-bearing organic matter is oxolane, ethanol or acetone；And, it is by silicon source, aluminum
After the mixing of source, it is blended into oxygen-bearing organic matter and water, stirring and evenly mixing obtains mixture at 15 DEG C～60 DEG C；
(2) prepare gel reaction mixture: at 10 DEG C～90 DEG C, be directed to agent and alkaline solution is added in silicon source, stir 1
～80h, adds silicon source, stirs, prepared gel reaction mixture；Wherein, the proportioning controlling gel reaction mixture is (1
～4) na2o:al2o3: (6～10) sio2: (100～300) h2O, and wherein directed agents consumption accounts for reactant mixture percentage by weight
1%～60%；
(3) the gel reaction mixture of preparation is warming up to 80～120 DEG C of crystallization 10～70h, then through filtering, washing, be dried
Step is obtained nay zeolite product.
2. method according to claim 1 it is characterised in that silicon source described in step (1) be selected from Ludox, waterglass,
One of white carbon, sodium silicate, positive silicic acid or multiple；Source of aluminium is selected from sodium metaaluminate, aluminum sulfate, aluminum nitrate or plan
One or more of boehmite.
3. method according to claim 2 is it is characterised in that silicon source described in step (1) is waterglass.
4. method according to claim 2 is it is characterised in that silicon source described in step (1) is sodium metaaluminate.
5. method according to claim 1 is it is characterised in that be directed to agent in step (2) and alkaline solution is added to silicon
Stirring 1h～50h after in source.
6. the method according to claim 1 or 5 is it is characterised in that be to prepare to coagulate at 10 DEG C～70 DEG C in step (2)
Glue reactant mixture.
7. the method according to claim 1 or 5 is it is characterised in that alkaline solution described in step (2) is sodium hydroxide
In solution, ammonia, sodium bicarbonate solution, sodium aluminate solution one or more.
8. method according to claim 1 it is characterised in that silicon source described in step (2) be selected from Ludox, waterglass,
One of white carbon, sodium silicate, positive silicic acid or multiple, source of aluminium is selected from sodium metaaluminate, aluminum sulfate, aluminum nitrate or plan
One or more of boehmite.
9. method according to claim 1 it is characterised in that in step (2) directed agents consumption account for reactant mixture weight
1%～20%.
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| RU2627900C1 (en) * | 2016-12-05 | 2017-08-14 | Федеральное государственное бюджетное учреждение науки Институт проблем переработки углеводородов Сибирского отделения Российской академии наук (ИППУ СО РАН) | Method of preparing microcrystalline nay zeolite |
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