CN105417553A - NaY molecular sieve and preparation method thereof - Google Patents
NaY molecular sieve and preparation method thereof Download PDFInfo
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- CN105417553A CN105417553A CN201410474786.0A CN201410474786A CN105417553A CN 105417553 A CN105417553 A CN 105417553A CN 201410474786 A CN201410474786 A CN 201410474786A CN 105417553 A CN105417553 A CN 105417553A
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Abstract
The invention discloses a preparation method for an NaY molecular sieve. The method comprises the steps of: roasting kaolin; and performing a crystallization reaction on the roasted product, a silicon source and a guiding agent. The method is characterized in that silicon source contains a silicon-containing filtrate which is obtained by contacting a silicon-containing filtrate of the NaY molecular sieve with an alkaline compound, so that the content of the NaY molecular sieve microcrystals in the silicon-containing filtrate is less than 0.005 wt%. The invention further discloses a NaY molecular sieve prepared by the method. By adopting the method disclosed by the invention, the contacted silicon-containing filtrate is used as the silicon source for preparing the NaY molecular sieve, so that the utilization of silicon is improved, the production cost is lowered, and discharge of a lot of silicon-containing filtrate and the environmental pollution are further avoided.
Description
Technical field
The present invention relates to a kind of NaY molecular sieve and preparation method thereof.
Background technology
NSY molecular sieve is a kind of Novel Y-shaped molecular sieves compound material with double-pore structure, it provides part " silicon source " and whole " aluminium source " with the kaolin of high-temperature roasting process, hydrothermal crystallizing is carried out in alkaline system Extra Section silicon source, in this in-situ crystallization reaction process, the part SiO in kaolin
2enter people's liquid phase, abundant macropore is formed at kaolin surface, NaY molecular sieve crystal growth is at kaolinic outside surface and inner surfaces of pores, thus form with kaolin the Y zeolite (also becoming NSY molecular sieve) of the double-pore structure being carrier, add catalyzer to reactant accessibility and catalytic activity.In actual production process, in order to improve the silica alumina ratio of product, the silica alumina ratio often fed intake is higher than the silica alumina ratio of product, therefore, when qualified NaY molecular sieve carries out filtration washing, the siliceous filtrate of a large amount of NaY molecular sieve will be produced, direct blowdown, both silicon can have been caused to run off, and cost raises, and can cause environmental pollution again.The siliceous filtrate that conventional NaY molecular sieve preparation produces, the siliceous filtrate of reuse is normally adopted first to prepare alumino silica gel, and using this alumino silica gel as part " silicon source " and " aluminium source " for the synthesis of NaY molecular sieve, thus reuse is carried out to the Si in the siliceous filtrate of NaY molecular sieve.But the siliceous filtrate recycle mode of this NaY molecular sieve both increased production cost, again due to the feature limits of technique own, cannot realize the fully recovering of filtrate silicon.
Summary of the invention
Object of the present invention overcomes the production cost existed in the reuse mode of the siliceous filtrate of existing NaY molecular sieve and realizes the defect of the silicon fully recovering in this filtrate with being difficult to, there is provided a kind of cost lower, and can realizing the method preparing NaY molecular sieve of the silicon fully recovering of siliceous for NaY molecular sieve filtrate, and NaY molecular sieve obtained by this method.
The present inventor is found by further investigation, owing to containing a large amount of NaY molecular sieve crystallites in the siliceous filtrate of NaY molecular sieve, if directly siliceous for NaY molecular sieve filtrate is carried out reuse as the silicon source of synthesis NaY molecular sieve, will have a strong impact on the synthesis of NaY molecular sieve, and the stuctures and properties of gained NaY molecular sieve is poor.Based on this discovery, the present inventor is by contacting siliceous for NaY molecular sieve filtrate with basic cpd, and make in the siliceous filtrate of NaY molecular sieve hardly containing NaY molecular sieve crystallite, thus the siliceous filtrate of NaY molecular sieve after contact can not only be effective as silicon source and prepare NaY molecular sieve, achieve the fully recovering in silicon source, and the NaY molecular sieve obtained have degree of crystallinity high, there is the excellent performance such as diplopore, high silica alumina ratio.
To achieve these goals, the invention provides a kind of preparation method of NaY molecular sieve, the method comprises: kaolin is carried out roasting, and the product after roasting and silicon source, directed agents are carried out crystallization, wherein, siliceous filtrate is contained in described silicon source, and described siliceous filtrate obtains by siliceous for NaY molecular sieve filtrate and basic cpd being carried out contacting, and described contact makes the NaY molecular sieve crystallite in described siliceous filtrate be less than 0.005 % by weight.
Present invention also offers the NaY molecular sieve obtained by aforesaid method.
By adopting method of the present invention, using the siliceous filtrate after described contact as silicon source for the preparation of NaY molecular sieve, the utilization ratio that improve silicon reduces production cost, also avoid the outer row of a large amount of siliceous filtrate and the pollution to environment.
Other features and advantages of the present invention are described in detail in embodiment part subsequently.
Embodiment
Below the specific embodiment of the present invention is described in detail.Should be understood that, embodiment described herein, only for instruction and explanation of the present invention, is not limited to the present invention.
The invention provides a kind of preparation method of NaY molecular sieve, the method comprises: kaolin is carried out roasting, and the product after roasting and silicon source, directed agents are carried out crystallization, wherein, siliceous filtrate is contained in described silicon source, described siliceous filtrate obtains by siliceous for NaY molecular sieve filtrate and basic cpd being carried out contacting, and described contact makes the NaY molecular sieve crystallite in described siliceous filtrate be less than 0.005 % by weight.
According to the present invention, in order to the NaY molecular sieve of excellent, usually can by described kaolin before carrying out roasting, adopt the method for this area routine to be prepared into kaolin microsphere, such as, first kaolin and water are made slurry, then spray shaping is microballoon (granularity of microballoon is such as 1-100 μm), the present invention is not particularly limited described kaolin, can be the kaolin product of commercially available various routines, under preferable case, with SiO in described kaolin microsphere
2the content of the element silicon of meter is 45-55 % by weight, with Al
2o
3the content of the aluminium element of meter is 42-48 % by weight.
According to the present invention, the roasting condition of described kaolin microsphere is not particularly limited, the kaolin roasting method of this area routine when preparing NaY molecular sieve can be adopted, in order to make the kaolinic activity after roasting higher, under preferable case, the condition of described roasting comprises: temperature is 600-900 DEG C, and the time is 2.5-3.5h.
According to the present invention, the product after roasting and silicon source, directed agents are carried out crystallization, NaY molecular sieve of the present invention can be obtained.Described crystallization can carry out in water, and under preferable case, the condition of described crystallization comprises: pH is 12-13, and temperature is 90-96 DEG C, and the time is 30-45h.More preferably, the condition of described crystallization comprises: pH is 12-12.5, and temperature is 92-96 DEG C, and the time is 30-40h.Wherein, pH is that the alkaline condition of 12-13 (be preferably 12-12.5) is regulated by the acting in conjunction of sodium hydroxide, water glass and directed agents.
According to the present invention, in order to obtain excellent NaY type molecular sieve, under preferable case, the consumption in described kaolin microsphere and described silicon source makes the mol ratio of element silicon and aluminium element be 5-6:1, more preferably 5.2-5.8:1.
According to the present invention, in order to make the better in-situ crystallization of kaolin obtain NaY molecular sieve, under preferable case, in the reaction system of described crystallization, the consumption in described kaolin and described silicon source makes with SiO
2the content of the element silicon of meter is 18-30 % by weight, with Al
2o
3the content of the aluminium element of meter is 2-6 % by weight.The content of the content (or aluminium element) of element silicon here refers in the reaction system of crystallization in position, and element silicon (or aluminium element) accounts for the weight percentage of the total amount of the material in whole reaction system.
In the present invention, siliceous filtrate is contained in described silicon source, and described siliceous filtrate is for obtaining by siliceous for NaY molecular sieve filtrate and basic cpd being carried out contacting.Described silicon source can be all siliceous filtrate, or part be siliceous filtrate, preferably, with the molar weight of the element silicon in described silicon source for benchmark, in described silicon source contain 0.5-80 % by mole in the siliceous filtrate of element silicon.More preferably in described silicon source containing 0.6-20 % by mole in the siliceous filtrate of element silicon.When the part in described silicon source is siliceous filtrate, remaining part silicon source can adopt the silicon source of this area routine, such as water glass, alumino silica gel etc.
In the present invention, described siliceous filtrate can be the solution after directly siliceous for NaY molecular sieve filtrate being contacted with basic cpd, element silicon in described siliceous filtrate and the content of aluminium element determined by the content of the element silicon in the siliceous filtrate of NaY molecular sieve and aluminium element, and those skilled in the art should understand is, element silicon in the siliceous filtrate of usual NaY molecular sieve and the content of aluminium element lower, therefore, when direct solution after siliceous for NaY molecular sieve filtrate contacts with basic cpd is used for as part silicon source as described siliceous filtrate time, it can not meet the needs of the mol ratio of element silicon and aluminium element when preparing NaY molecular sieve of the present invention, therefore, generally, need to adopt the silicon source of this area routine as supply silicon source, such as water glass, alumino silica gel etc.But in this case, due to direct part silicon source solution after siliceous for NaY molecular sieve filtrate contacts with basic cpd is used for as described siliceous filtrate as preparation NaY molecular sieve, particularly carrying out on a large scale, in the suitability for industrialized production of multiple retort simultaneous reactions, a large amount of NaY molecular sieve can be used siliceous filtrate, and without the need to spending a large amount of time to process it, can while the utilization ratio of the silicon increased, decrease the quantity discharged of siliceous filtrate waste water, for large-scale industrial production, there is beyond thought economic benefit.
As mentioned above, the siliceous filtrate of above-mentioned NaY molecular sieve of the present invention can directly use as the part silicon source of preparing NaY molecular sieve as described siliceous filtrate after contacting with described basic cpd, but also can the siliceous filtrate of above-mentioned NaY molecular sieve after contacting with described basic cpd, carry out again heating concentrated obtain element silicon content and the higher siliceous filtrate of the content of the aluminium element part or all of silicon source that is re-used as preparation NaY molecular sieve use, but reduce costs aspect for save energy to consider, preferably direct the solution of siliceous for NaY molecular sieve filtrate after contacting with described basic cpd to be used as described siliceous filtrate as the part silicon source of preparing NaY molecular sieve.
Owing to containing a certain amount of NaY molecular sieve crystallite in the siliceous filtrate of NaY molecular sieve, therefore, the present invention is by siliceous for described NaY molecular sieve filtrate and basic cpd being carried out contacting the liquid obtained as the siliceous filtrate in silicon source.By siliceous for NaY molecular sieve filtrate being contacted with basic cpd, the NaY molecular sieve crystallite contained in filtrate almost dissolves completely, is less than 0.005 % by weight.Preferably, described contact makes in described siliceous filtrate completely not containing NaY molecular sieve crystallite.Thus the NaY molecular sieve crystallite avoided owing to containing in siliceous filtrate causes bad impact to NaY molecular sieve synthesis.
NaY molecular sieve crystallite contained in the siliceous filtrate of NaY molecular sieve be due to portions microcrystalline during product after washing crystallization with water from wash-out microballoon and the crystallite of people's filtrate can be entered, the granularity of such as described NaY molecular sieve crystallite can be below 500nm, is preferably 500-200nm.To the amount of described NaY molecular sieve crystallite, also there is no particular limitation in the present invention, and its content is determined by the situation of filtering, and such as the amount of described NaY molecular sieve crystallite is 1-5 % by weight.
Why the siliceous filtrate of NaY molecular sieve can be used as silicon source after contacting with basic cpd, be that it contains a certain amount of element silicon and aluminium element, and be filtered by crystallization and obtain, other impurity element can not be substituted into again, in the present invention, the amount of the element silicon contained in the siliceous filtrate of NaY molecular sieve and aluminium element is not particularly limited, as long as NaY molecular sieve can be prepared as silicon source, the content of the element silicon such as, contained in the siliceous filtrate of described NaY molecular sieve is 0.09-0.15 % by weight, the content of aluminium element is 0.025-0.04 % by weight.
According to the present invention, under preferable case, the siliceous filtrate of described NaY molecular sieve and basic cpd carry out contacting condition comprise: temperature is 90-96 DEG C, and the time is 2-4.Preferably, described basic cpd is sodium hydroxide and/or sodium methylate, is more preferably sodium hydroxide.
According to the present invention, described NaY molecular sieve siliceous filtrate is not particularly limited the consumption of described basic cpd when contacting with described basic cpd, as long as the NaY molecular sieve crystallite in described siliceous filtrate can be made to be less than 0.005 % by weight (very micro-, not can to think and contain).Under preferable case, in the weight ratio of the NaY molecular sieve crystallite in the siliceous filtrate of the NaY molecular sieve of element silicon and described basic cpd for 1:0.08-0.1, more preferably 1:0.08-0.09.
According to the present invention, described crystallization is kaolin in-situ crystallization reaction.Wherein, need to add directed agents.The present invention is not particularly limited described directed agents, as long as the carrying out of crystallization can be brought out as the crystal seed of NaY molecular sieve, under preferable case, described directed agents in mole chemical expression be: (12-16) SiO
2al
2o
3(14-18) Na
2o (300-350) H
2o.
In addition, in the present invention, also having no particular limits the consumption of described directed agents, can be the conventional amount used of this area.Under preferable case, for the product after the roasting of 100 weight parts, the consumption of described directed agents is 40-60 weight part.
According to the present invention, under preferable case, the method also comprises: wash the product after described crystallization with water and solid-liquid separation, and solid-liquid separation gained liquid phase is used as the siliceous filtrate of described NaY molecular sieve.Namely, to have employed after siliceous filtrate carries out above-mentioned crystallization as silicon source (part or whole), the products in water of crystallization is carried out washing and solid-liquid separation, solid-liquid separation gained liquid phase is also the siliceous filtrate of a kind of NaY molecular sieve, reuses after may be used for equally contacting with basic cpd as silicon source.
Present invention also offers and prepared by aforesaid method and the NaY molecular sieve obtained.
Below will be described the present invention by embodiment.
In following preparation example, embodiment and comparative example,
NaY molecular sieve content in solids product and siliceous filtrate according to RIPP146-90 standard method (see " Petrochemical Engineering Analysis method " (RIPP test method), Yang Cui delimits the organizational structure, Science Press, nineteen ninety publishes) measure, wherein, be less than detectability to be namely less than 0.005 % by weight and to be considered to 0 % by weight;
The quality product situation of the NaY molecular sieve in solids product is undertaken analyzing by the distribution situation measuring NaY molecular sieve crystal according to X-ray diffractometer.
Preparation example 1
This preparation example is for illustration of the preparation method of siliceous filtrate of the present invention.
(granularity is 2 μm, with SiO kaolin to be made kaolin microsphere
2the content of the element silicon of meter is 50 % by weight, with Al
2o
3the content of the aluminium element of meter is 45 % by weight), then roasting 3h at 700 DEG C, by the directed agents (14SiO of the water glass of the product after 100g roasting, 453g, 50g
21Al
2o
317Na
2o300H
2o) and 24 % by weight aqueous sodium hydroxide solutions of 54g join in the water of 500mL and (make pH be 12.2), in-situ crystallization reaction 28h at 93 DEG C; With the product after 500ml water washing crystallization and solid-liquid separation, gained solid phase 556g, wherein the content of NaY molecular sieve is 74.5 % by weight, and according to X-ray diffractometer by measuring the distribution situation of NaY molecular sieve crystal, its quality product is qualified; Gained liquid phase is that 1000g is the siliceous filtrate of NaY molecular sieve, and wherein the content of NaY molecular sieve crystallite is 1.3 % by weight, and granularity is below 500nm, and the content of element silicon is 0.99 % by weight, and the content of aluminium element is 0.31 % by weight.
In the siliceous filtrate of above-mentioned NaY molecular sieve, add 1.07g sodium hydroxide, contact reacts 3h at 95 DEG C, make the content of the NaY molecular sieve crystallite in the siliceous filtrate of NaY molecular sieve be 0 % by weight, thus obtain siliceous filtrate A1.
Embodiment 1
The present embodiment prepares the method for NaY molecular sieve and obtained NaY molecular sieve thereof for illustration of kaolin in-situ crystallization of the present invention.
(granularity is 2 μm, with SiO kaolin to be obtained kaolin microsphere
2the content of the element silicon of meter is 50 % by weight, with Al
2o
3the content of the aluminium element of meter is 45 % by weight), then roasting 3h at 700 DEG C, by the water glass of siliceous filtrate A1,450g of the product after 100g roasting, 100g preparation example 1 gained, the directed agents (14SiO of 50g
21Al
2o
317Na
2o300H
2o) and 20 % by weight aqueous sodium hydroxide solutions of 5.8g join in the water of 350mL and (make pH be 12.5), in-situ crystallization reaction 28h at 93 DEG C; With the product after 400ml water washing crystallization and solid-liquid separation, gained solid phase 557g, wherein the content of NaY molecular sieve is 73.6 % by weight, and according to X-ray diffractometer by measuring the distribution situation of NaY molecular sieve crystal, its quality product is qualified; Gained liquid phase (820g) is the siliceous filtrate of NaY molecular sieve, and wherein the content of NaY molecular sieve crystallite is 1.5 % by weight, and granularity is below 500nm, and the content of element silicon is 0.97 % by weight, and the content of aluminium element is 0.3 % by weight.
In the siliceous filtrate of this NaY molecular sieve, add 1g sodium hydroxide, contact reacts 2.5h at 96 DEG C, make the content of the NaY molecular sieve crystallite in the siliceous filtrate of NaY molecular sieve be 0 % by weight, thus obtain siliceous filtrate A2.
Embodiment 2
The present embodiment prepares the method for NaY molecular sieve and obtained NaY molecular sieve thereof for illustration of kaolin in-situ crystallization of the present invention.
(granularity is 10 μm, with SiO kaolin to be obtained kaolin microsphere
2the content of the element silicon of meter is 50 % by weight, with Al
2o
3the content of the aluminium element of meter is 45 % by weight), then roasting 2.5h at 800 DEG C, by the water glass of siliceous filtrate A2,445g of the product after 100g roasting, 200g embodiment 1 gained, the directed agents (15SiO of 50g
2al
2o
315Na
2o350H
2o) and 30 % by weight aqueous sodium hydroxide solutions of 4g join in the water of 200mL and (make pH be 12), in-situ crystallization reaction 25h at 95 DEG C; With the product after 500ml water washing crystallization and solid-liquid separation, gained solid is 561g, and wherein the content of NaY molecular sieve is 73.2 % by weight, and according to X-ray diffractometer by measuring the distribution situation of NaY molecular sieve crystal, its quality product is qualified; Gained liquid phase (840g) is the siliceous filtrate of NaY molecular sieve, and wherein the content of NaY molecular sieve crystallite is 1.43 % by weight, and granularity is below 500nm, and the content of element silicon is 0.98 % by weight, and the content of aluminium element is 0.33 % by weight.
Embodiment 3
The present embodiment prepares the method for NaY molecular sieve and obtained NaY molecular sieve thereof for illustration of kaolin in-situ crystallization of the present invention.
(granularity is 8 μm, with SiO kaolin to be obtained kaolin microsphere
2the content of the element silicon of meter is 50 % by weight, with Al
2o
3the content of the aluminium element of meter is 45 % by weight), then roasting 3h at 850 DEG C, by (concentrated through heating for the siliceous filtrate A1 of the product after 100g roasting, 100g, make the content of element silicon be 12 % by weight, the content of aluminium element is 3.5 % by weight), 430g water glass, 60g directed agents (16SiO
2al
2o
316Na
2o340H
2o) and 25 % by weight aqueous sodium hydroxide solutions of 6g join in 400mL water and (make pH be 12.3), in-situ crystallization reaction 30h at 94 DEG C; With the product after 500ml water washing crystallization and solid-liquid separation, gained solid phase is the content of NaY molecular sieve in 547g is 75.1 % by weight, and according to X-ray diffractometer by measuring the distribution situation of NaY molecular sieve crystal, its quality product is qualified; Gained liquid phase (950g) is the siliceous filtrate of NaY molecular sieve, and wherein the content of NaY molecular sieve crystallite is 1.37 % by weight, and granularity is below 500nm, and the content of element silicon is 0.92 % by weight, and the content of aluminium element is 0.27 % by weight.
In the siliceous filtrate of above-mentioned NaY molecular sieve, add 1.1g sodium hydroxide, contact reacts 4h at 90 DEG C, make the content of the NaY molecular sieve crystallite in the siliceous filtrate of NaY molecular sieve be 0 % by weight, thus obtain siliceous filtrate A3.
Comparative example 1
Method according to embodiment 1, difference is, adds 9 % by weight alum liquors of 2g in the siliceous filtrate of NaY molecular sieve of 100g, the alumino silica gel of obtained 1.2g, in residual solution, the content of element silicon is 0.75 % by weight, and the content of aluminium element is 1.5 % by weight; Instead siliceous for this alumino silica gel filtrate is carried out crystallization as part silicon source, gained solid phase 548g, wherein the content of NaY molecular sieve is 73.5 % by weight, and according to X-ray diffractometer by measuring the distribution situation of NaY molecular sieve crystal, its quality product is qualified; Gained liquid phase (750g) is the siliceous filtrate of NaY molecular sieve, and wherein the content of NaY molecular sieve crystallite is 2.3 % by weight, and granularity is below 500nm, and the content of element silicon is 1.34 % by weight, and the content of aluminium element is 0.6 % by weight.
Comparative example 2
Method according to embodiment 1, difference is, directly siliceous for the NaY molecular sieve of 100g filtrate is carried out crystallization as silicon source, in gained solid phase (545g), the content of NaY molecular sieve is 72.5 % by weight, but product caking is serious, present uneven dispersion, off quality; Gained liquid phase (825g) is the siliceous filtrate of NaY molecular sieve, and wherein the content of NaY molecular sieve crystallite is 1.8 % by weight, and granularity is below 500nm, and the content of element silicon is 1.1 % by weight, and the content of aluminium element is 0.37 % by weight.
Known by above-described embodiment, adopt method of the present invention to be prepared NaY molecular sieve, the utilization ratio of the Silicified breccias in siliceous filtrate can be improved.
In addition, when adopting method of the present invention to be prepared NaY molecular sieve, produce molecular sieve per ton and can save fresh water more than 5 tons, reduce externally discharged waste water more than 5 tons.
More than describe the preferred embodiment of the present invention in detail; but the present invention is not limited to the detail in above-mentioned embodiment, within the scope of technical conceive of the present invention; can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.
It should be noted that in addition, each concrete technical characteristic described in above-mentioned embodiment, in reconcilable situation, can be combined by any suitable mode, in order to avoid unnecessary repetition, the present invention illustrates no longer separately to various possible array mode.
In addition, also can carry out arbitrary combination between various different embodiment of the present invention, as long as it is without prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (14)
1. the preparation method of a NaY molecular sieve, the method comprises: kaolin is carried out roasting, and the product after roasting and silicon source, directed agents are carried out crystallization, it is characterized in that, siliceous filtrate is contained in described silicon source, described siliceous filtrate obtains by siliceous for NaY molecular sieve filtrate and basic cpd being carried out contacting, and described contact makes the NaY molecular sieve crystallite in described siliceous filtrate be less than 0.005 % by weight.
2. method according to claim 1, wherein, with the molar weight of the element silicon in described silicon source for benchmark, in described silicon source containing 0.5-80 % by mole in the siliceous filtrate of element silicon.
3. method according to claim 1, wherein, the consumption in described kaolin and described silicon source makes the mol ratio of element silicon and aluminium element be 5-6:1, preferred 5.2-5.8:1.
4. the method according to claim 1 or 3, wherein, in the reaction system of described crystallization, the consumption in described kaolin and described silicon source makes with SiO
2the content of the element silicon of meter is 18-30 % by weight, with Al
2o
3the content of the aluminium element of meter is 2-6 % by weight.
5. method according to claim 1, wherein, described basic cpd is sodium hydroxide and/or sodium methylate.
6. method according to claim 1, wherein, the NaY molecular sieve crystallite in the siliceous filtrate of described NaY molecular sieve and the weight ratio of described basic cpd are 1:0.08-0.1, preferred 1:0.08-0.09.
7. method according to claim 1, wherein, described directed agents in mole chemical expression be: (12-16) SiO
2al
2o
3(14-18) Na
2o (300-350) H
2o.
8. method according to claim 1, wherein, relative to the product after the roasting of 100 weight parts, the consumption of described directed agents is 40-60 weight part.
9. according to the method in claim 1-8 described in any one, wherein, the content of the element silicon in the siliceous filtrate of described NaY molecular sieve is 0.09-0.15 % by weight, and the content of aluminium element is 0.025-0.04 % by weight.
10. method according to claim 1, wherein, the condition of described crystallization comprises: pH is 12-13, and temperature is 90-96 DEG C, and the time is 30-45h.
11. methods according to claim 1, wherein, the condition that siliceous for described NaY molecular sieve filtrate and described basic cpd carry out contacting comprised: temperature is 90-96 DEG C, the time is 2-4h.
12. methods according to claim 1, wherein, the condition of described roasting comprises: temperature is 600-900 DEG C, and the time is 2.5-3.5h.
13. methods according to claim 1, wherein, the method also comprises: wash the product after described crystallization with water and solid-liquid separation, and solid-liquid separation gained liquid phase is used as the siliceous filtrate of described NaY molecular sieve.
14. NaY molecular sieve obtained by the method preparation in claim 1-13 described in any one.
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| CN114715909A (en) * | 2021-01-06 | 2022-07-08 | 中国石油天然气股份有限公司 | Kaolin in-situ synthesized small-grain NaY molecular sieve and preparation method thereof |
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| 周继红: "合成分子筛母液及其利用研究", 《现代化工》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114715909A (en) * | 2021-01-06 | 2022-07-08 | 中国石油天然气股份有限公司 | Kaolin in-situ synthesized small-grain NaY molecular sieve and preparation method thereof |
| CN114715909B (en) * | 2021-01-06 | 2023-05-26 | 中国石油天然气股份有限公司 | Kaolin in-situ synthesized small-grain NaY molecular sieve and preparation method thereof |
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| CN105417553B (en) | 2018-04-13 |
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