CN106745044B - One kind uses Na2CO3The method for aiding in synthesizing low silicon aluminum ratio X-type molecular sieve - Google Patents
One kind uses Na2CO3The method for aiding in synthesizing low silicon aluminum ratio X-type molecular sieve Download PDFInfo
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Abstract
The present invention relates to inorganic material molecular sieve powder preparing technical field, it is desirable to provide a kind of method for widening low silica-alumina ratio X-type zeolite molecular sieve synthesis scope.This method is specifically that one kind uses Na2CO3The method for aiding in synthesizing low silicon aluminum ratio X-type molecular sieve, comprises the following steps：（1）Prepare directed agents：Silicon source is added in silicon source, alkali source and water, prepares directed agents；（2）Synthesizing low silicon aluminum ratio X-type molecular sieve original powder is aided in using Na2CO3.By the present invention in that use Na2CO3Auxiliary has synthesized pure phase and the preferable low silica-alumina ratio X-type molecular sieve of crystallinity；The Na2CO3 raw materials of use are the corrosivity raw materials of industry that is weaker, cheap and easy to get, being adapted to large-scale production and application；The alkalescence of especially Na2CO3 raw materials is weaker, and the stabilization of basicity can be kept in broader synthetic ratio opereating specification, realizes the fine modulation of reaction system basicity.
Description
Technical field
The present invention relates to inorganic material-molecular sieve powder preparing technical field, is specifically that one kind uses Na2CO3Auxiliary synthesis
The method of low silica-alumina ratio X-type molecular sieve.
Background technology
Low silica-alumina ratio X-type molecular sieve is a kind of molecular sieve with cube faujasite structure, silica alumina ratio n (SiO2)/n
(Al2O3)=2.0~2.2.Low silica-alumina ratio X-type molecular sieve passes through Li+The Li-LSX type molecular sieves of high exchange degree are exchanged for, are had
Larger N2 adsorption capacity and nitrogen oxygen separating coefficient, absorption property is more excellent, be currently in pressure swing adsorption method making oxygen by air separation technology most
For preferable adsorbent；Further, since n (the SiO of LSX type molecular sieves2)/n(Al2O3) low, tradable cation-bit is therewith
Increase possibly even reaches maximum, and it is used as the performance of detergent builders also superior to 4A type molecular sieves, as catalyst or urges
Agent carrier is also bigger than common X-type molecular sieve to the modulation scope of catalytic performance, and therefore, low silica-alumina ratio X-type molecular sieve is in industry
On have a wide range of applications.
The lot of domestic and international document report synthetic method of low silica-alumina ratio X-type molecular sieve, but due in sodium potassium system
The synthesis of low silica-alumina ratio X-type molecular sieve is to n (H2O/NaK change) is very sensitive, and scale is more general than excursion in synthetic ratio
All over very little [n (H2O/NaK)=16~17], changed in the range of can only being about 1 in width, A types and S will be caused by being off slightly from
The generation of type zeolite stray crystal phase, therefore the formula synthesis scope of low silica-alumina ratio X-type molecular sieve is narrower, it is extremely easy in preparation process
Stray crystal phase is generated, synthesis difficulty is larger, and the molecular sieve powder that high-purity is made is difficult to when especially mass producing.
The content of the invention
Scale ratio excursion is small in being matched present invention aim to address low silica-alumina ratio X-type molecular sieve, molecular sieve is matched somebody with somebody
Fang Hecheng narrow ranges, the problem of difficulty is big is prepared, to solve the above problems, the invention provides one kind to use Na2CO3Auxiliary is closed
Into the method for low silica-alumina ratio X-type molecular sieve.
The present invention is achieved by the following technical solutions：One kind uses Na2CO3Aid in synthesizing low silicon aluminum ratio X type molecules
The method of sieve, comprises the following steps：
(1) directed agents are prepared：Silicon source is added in silicon source, alkali source and water, prepares directed agents；
(2) Na is used2CO3Aid in synthesizing low silicon aluminum ratio X-type molecular sieve original powder：
A, stock up
It is in molar ratio:SiO2/Al2O3=1.9~2.3, Na2O/(Na2O+K2O)=0.73~0.8, H2O/SiO2=50
~69, H2O/(Na2O+K2)=11~16, O wherein Na2CO3/Na2The ratio of O=0.3~0.7 feeds intake, and measures respective amount respectively
Silicon source, silicon source, alkali source and water as raw material；
B, plastic
Silicon source, alkali source and water are added in reactor successively under agitation, mixes to and is completely dissolved, Ran Hou
Silicon source is added under stirring, 0.5~1h is stirred under room temperature condition, obtains mixture material, finally add in mixture material
Enter the directed agents of 3%~5% mass percent, stir 0.5~1h at ambient temperature and carry out plastic；
C, aging and crystallization
After the completion of plastic, by mixture gel at 60~70 DEG C 8~22h of static burn in；After aging terminates, then will mixing
Thing gel is placed in 3~4h of static crystallization at 100 DEG C；
D, it is filtered, washed and dried
After the completion of crystallization, slurry is separated into solid molecular sieves and mother liquor, solid product is washed with water to neutrality, in 100
Dry, produced using Na at DEG C2CO3Aid in the low silica-alumina ratio X-type molecular sieve of synthesis.
Further, step (1) prepares the method for directed agents including being：First silicon source and alkali source are added to the water and stirred to complete
Dissolving obtains high alkalinity sodium aluminate solution, and then silicon source is slowly added into high alkalinity sodium aluminate, after stirring at room temperature,
15 DEG C~30 DEG C 8~16h of static placement, produce required directed agents；The mol ratio of each raw material is Na wherein in directed agents2O:SiO2:
Al2O3:H2O=17:5.76:1:250.
Further, the alkali source in step (1) is solid sodium hydroxide or sodium hydrate aqueous solution.
Further, the alkali source in described step (2) mixes for the solid of natrium carbonicum calcinatum, sodium hydroxide and potassium hydroxide
Thing, or three's mixture solution.
Further, the silicon source in step (1) and (2) is the aqueous solution of sodium metasilicate or sodium metasilicate.
Further, the silicon source in step (1) and (2) is the aqueous solution of sodium aluminate or sodium aluminate.
It is provided by the present invention to use Na2CO3Aid in synthesizing low silicon aluminum ratio X-type molecular sieve method compared with prior art,
Have the advantages that：
1st, the present invention is in the range of said ratio, using two one-step hydrothermals in sodium potassium system, adds directed agents, static old
Change and crystallization, SiO is finally made2/Al2O3Between mol ratio is 2.0~2.2, crystallite dimension is that the pure phase between 1~3 μm is low
Silica alumina ratio X-type molecular sieve.
2nd, the Na used in the present invention2CO3Raw material alkalescence is relatively weak, can be protected in broader synthetic ratio opereating specification
The stabilization of basicity is held, realizes the fine modulation of system basicity.So as to effectively widen the synthesis of low silica-alumina ratio X-type molecular sieve
Section, production difficulty is reduced, be advantageous to industrialized production improvement.
3rd, the Na used in the present invention2CO3Raw material is the raw material of industry that corrosivity is weaker, cheap and easy to get, reduces and is produced into
This.
Brief description of the drawings
Fig. 1 is the XRD spectrum of sample synthesized by embodiment 1 to 3.
Fig. 2 is the XRD spectrum of sample synthesized by embodiment 4 to 6.
Fig. 3 is the SEM figures of sample synthesized by embodiment 3.
Embodiment
Synthesized in embodiment using two one-step hydrothermals, with sodium silicate solution (SiO2313g/L, Na2O 100g/L) it is silicon
Source, with sodium aluminate (Al2O341%, Na2O 35%) it is silicon source, with sodium carbonate (Na2CO399.8%), sodium hydroxide (NaOH
96%), potassium hydroxide (KOH 85%) is sodium potassium basic materials, a series of molecular sieve samples of static monitor in stainless steel cauldron
Product.
Embodiment 1：
One kind uses Na2CO3The method for aiding in synthesizing low silicon aluminum ratio X-type molecular sieve, specifically includes following steps：
(1) directed agents are prepared
Under agitation successively by 1.382g sodium aluminate solids (Al2O30.0056mol, Na2O 0.0078mol)、
6.396g sodium hydroxides (0.0768mol) are added in 18.6ml deionized waters, obtain high alkalinity sodium aluminate solution, then will
6.4ml sodium silicate solutions (SiO20.032mol, Na2O 0.01mol) it is slowly added in high alkalinity sodium aluminate solution, at room temperature
0.5h is stirred, it is directed agents to stand under the conditions of 25 DEG C after aging 9h. Na2O:SiO2:Al2O3:H2O=0.0946:0.032:
0.0056:1.3889=17:5.76:1:250, the calculating of the amount of the material of its reclaimed water is：(6.4+18.6)/18=
1.3889mol。
(2) Na is used2CO3Aid in synthesizing low silicon aluminum ratio X-type molecular sieve original powder
Under agitation successively by 2.488g sodium aluminates (Al2O30.0100mol, Na2O 0.0140mol)、 5.069g
Natrium carbonicum calcinatum (Na2CO30.0477mol, Na2O 0.0477mol), 2.292g solid sodium hydroxides (Na2O
0.0275mol), 3.144g solid potassium hydroxides (K2O 0.0239mol) add 19.8ml (H2O 1.1000mol) deionized water
Middle stirring is then slowly added into 3.83ml sodium silicate solutions (SiO to being completely dissolved20.0200mol, Na2O 0.0062mol),
0.5h is stirred at room temperature, is eventually adding the directed agents for accounting for reactant gross mass 4%, continues to stir 0.5h under room temperature condition；Will be anti-
Answer thing the static burn in 8h at 60 DEG C, the static crystallization 3h at 100 DEG C；After the completion of crystallization, slurry is separated into solid molecular sieves
And mother liquor, solid product are washed with water to neutrality, dried at 100 DEG C, product is produced after the completion of drying.Obtained product
XRD spectrum, silica alumina ratio and relative crystallinity are shown in Fig. 1 and table 1.
The mol ratio of each raw material is in step (2):SiO2/Al2O3=2, Na2O/(Na2O+K2O)=0.8, H2O/SiO2=
65.6,H2O/(Na2O+K2O)=11, Na2CO3/Na2O=0.5.
Embodiment 2：
One kind uses Na2CO3The method of synthesizing low silicon aluminum ratio X-type molecular sieve, specifically includes following steps：
(1) directed agents are prepared
1.382g sodium aluminate solids, 6.396g sodium hydroxides are added into 18.6ml deionized waters successively under agitation
In, high alkalinity sodium aluminate solution is obtained, then 6.4ml sodium silicate solutions are slowly added in high alkalinity sodium aluminate solution, in room
Temperature lower stirring 0.5h, it is directed agents to stand under the conditions of 25 DEG C after aging 10h.
(2) Na is used2CO3Aid in synthesizing low silicon aluminum ratio X-type molecular sieve original powder
Under agitation successively by 2.488g sodium aluminates (Al2O30.0100mol, Na2O 0.0140mol)、 4.559g
Natrium carbonicum calcinatum (Na2CO30.0429mol, Na2O 0.0429mol), 1.893g solid sodium hydroxides (Na2O
0.0227mol), 3.099g solid potassium hydroxides (K2O 0.0235mol) add 19.8ml deionized waters (H2O 1.1000mol)
Middle stirring is then slowly added into 3.83ml sodium silicate solutions (SiO to being completely dissolved20.0200mol, Na2O 0.0062mol),
0.5h is stirred at room temperature, is eventually adding the directed agents for accounting for reactant gross mass 3%, continues to stir 0.5h under room temperature condition；Will be anti-
Answer thing the static burn in 10h at 60 DEG C, the static crystallization 3.5h at 100 DEG C；After the completion of crystallization, slurry is separated into molecular solids
Sieve and mother liquor, solid product are washed with water to neutrality, are dried at 100 DEG C, and product is produced after the completion of drying.Obtained product
XRD spectrum, silica alumina ratio and relative crystallinity are shown in Fig. 1 and table 1.
The mol ratio of each raw material is in step (2):SiO2/Al2O3=2, Na2O/(Na2O+K2O)=0.785, H2O/SiO2
=65.6, H2O/(Na2O+K2O)=12, Na2CO3/Na2O=0.5.
Embodiment 3：
One kind uses Na2CO3The method of synthesizing low silicon aluminum ratio X-type molecular sieve, specifically includes following steps：
(1) directed agents are prepared
1.382g sodium aluminate solids, 6.396g sodium hydroxides are added into 18.6ml deionized waters successively under agitation
In, high alkalinity sodium aluminate solution is obtained, then 6.4ml sodium silicate solutions are slowly added in high alkalinity sodium aluminate solution, in room
Temperature lower stirring 0.5h, it is directed agents to stand under the conditions of 30 DEG C after aging 8h.
(2) Na is used2CO3Aid in synthesizing low silicon aluminum ratio X-type molecular sieve original powder
Under agitation successively by 2.488g sodium aluminates, 4.129g natrium carbonicum calcinatums, 1.554g solid sodium hydroxides,
Stirred in 3.059g solid potassium hydroxides to being completely dissolved, be then slowly added into 3.83ml sodium silicate solutions, stir at room temperature
0.5h, the directed agents for accounting for reactant gross mass 4% are eventually adding, continue to stir 0.5h under room temperature condition；By reactant in 65 DEG C
Lower static burn in 10h, the static crystallization 4h at 100 DEG C；After the completion of crystallization, slurry is separated into solid molecular sieves and mother liquor, Gu
Body product is washed with water to neutrality, is dried at 100 DEG C, and product is produced after the completion of drying.The XRD spectrum of obtained product, SEM
Figure, silica alumina ratio and relative crystallinity are shown in Fig. 1, Fig. 3 and table 1.
The mol ratio of each raw material is in step (2):SiO2/Al2O3=2, Na2O/(Na2O+K2O)=0.77, H2O/SiO2
=65.6, H2O/(Na2O+K2O)=13, Na2CO3/Na2O=0.5.
Embodiment 4：
One kind uses Na2CO3The method of synthesizing low silicon aluminum ratio X-type molecular sieve, specifically includes following steps：
(1) directed agents are prepared
1.382g sodium aluminate solids, 6.396g sodium hydroxides are added into 18.6ml deionized waters successively under agitation
In, high alkalinity sodium aluminate solution is obtained, then 6.4ml sodium silicate solutions are slowly added in high alkalinity sodium aluminate solution, in room
Temperature lower stirring 0.5h, it is directed agents to stand under the conditions of 25 DEG C after aging 12h.
(2) Na is used2CO3Aid in synthesizing low silicon aluminum ratio X-type molecular sieve original powder
Under agitation successively by 2.488g sodium aluminates, 3.768g natrium carbonicum calcinatums, 1.272g solid sodium hydroxides,
Stirred in 3.003g solid potassium hydroxides to being completely dissolved, be then slowly added into 3.83ml sodium silicate solutions, stir at room temperature
0.5h, the directed agents for accounting for reactant gross mass 3% are eventually adding, continue to stir 0.5h under room temperature condition；By reactant in 60 DEG C
Lower static burn in 15h, the static crystallization 4h at 100 DEG C；After the completion of crystallization, slurry is separated into solid molecular sieves and mother liquor, Gu
Body product is washed with water to neutrality, is dried at 100 DEG C, and product is produced after the completion of drying.The XRD spectrum of obtained product, silicon
Aluminum ratio and relative crystallinity are shown in Fig. 2 and table 1.
The mol ratio of each raw material is in step (2):SiO2/Al2O3=2, Na2O/(Na2O+K2O)=0.757, H2O/SiO2
=65.6, H2O/(Na2O+K2O)=14, Na2CO3/Na2O=0.5.
Embodiment 5：
One kind uses Na2CO3The method of synthesizing low silicon aluminum ratio X-type molecular sieve, specifically includes following steps：
(1) directed agents are prepared
By known technology, 1.382g sodium aluminate solids, 6.396g sodium hydroxides are added successively under agitation
In 18.6ml deionized waters, high alkalinity sodium aluminate solution is obtained, 6.4ml sodium silicate solutions are then slowly added to high alkalinity aluminic acid
In sodium solution, 0.5h is stirred at room temperature, it is directed agents to be stood under the conditions of 28 DEG C after aging 9h.
(2) Na is used2CO3Aid in synthesizing low silicon aluminum ratio X-type molecular sieve original powder
Under agitation successively by 2.488g sodium aluminates, 3.452g natrium carbonicum calcinatums, 1.023g solid sodium hydroxides,
2.965g solid potassium hydroxides are added in 19.8ml deionized waters and stirred to being completely dissolved, and are then slowly added into 3.83ml sodium metasilicate
Solution, 0.5h is stirred at room temperature, be eventually adding the directed agents for accounting for reactant gross mass 5%, continue to stir 0.5h under room temperature condition；
By reactant at 70 DEG C static burn in 8h, the static crystallization 3h at 100 DEG C；After the completion of crystallization, slurry is separated into solid point
Son sieve and mother liquor, solid product are washed with water to neutrality, are dried at 100 DEG C, and product is produced after the completion of drying.Obtained product
XRD spectrum, silica alumina ratio and relative crystallinity see Fig. 2 and table 1.
The mol ratio of each raw material is in step (2):SiO2/Al2O3=2, Na2O/(Na2O+K2O)=0.743, H2O/SiO2
=65.6, H2O/(Na2O+K2O)=15, Na2CO3/Na2O=0.5.
Embodiment 6：
One kind uses Na2CO3The method of synthesizing low silicon aluminum ratio X-type molecular sieve, specifically includes following steps：
(1) directed agents are prepared
By known technology, 1.382g sodium aluminate solids, 6.396g sodium hydroxides are added successively under agitation
In 18.6ml deionized waters, high alkalinity sodium aluminate solution is obtained, 6.4ml sodium silicate solutions are then slowly added to high alkalinity aluminic acid
In sodium solution, 0.5h is stirred at room temperature, it is directed agents to be stood under the conditions of 20 DEG C after aging 12h.
(2) Na is used2CO3Aid in synthesizing low silicon aluminum ratio X-type molecular sieve original powder
Under agitation successively by 2.488g sodium aluminates, 3.186g natrium carbonicum calcinatums, 0.815g solid sodium hydroxides,
2.903g solid potassium hydroxides are added in 19.8ml deionized waters and stirred to being completely dissolved, and are then slowly added into 3.83ml sodium metasilicate
Solution, 1.0h is stirred at room temperature, be eventually adding the directed agents for accounting for reactant gross mass 4%, continue to stir 0.5h under room temperature condition；
By reactant at 60 DEG C static burn in 15h, the static crystallization 3.5h at 100 DEG C；After the completion of crystallization, slurry is separated into solid
Molecular sieve and mother liquor, solid product are washed with water to neutrality, are dried at 100 DEG C, and product is produced after the completion of drying.Obtained production
XRD spectrum, silica alumina ratio and the relative crystallinity of thing are shown in Fig. 2 and table 1.
The mol ratio of each raw material is in step (2):SiO2/Al2O3=2, Na2O/(Na2O+K2O)=0.731, H2O/SiO2
=65.6, H2O/(Na2O+K2O)=16, Na2CO3/Na2O=0.5.
Embodiment 7：
One kind uses Na2CO3The method of synthesizing low silicon aluminum ratio X-type molecular sieve, specifically includes following steps：
(1) directed agents are prepared
By known technology, 1.382g sodium aluminate solids, 6.396g sodium hydroxides are added successively under agitation
In 18.6ml deionized waters, high alkalinity sodium aluminate solution is obtained, 6.4ml sodium silicate solutions are then slowly added to high alkalinity aluminic acid
In sodium solution, 0.5h is stirred at room temperature, it is directed agents to be stood under the conditions of 15 DEG C after aging 15h.
(2) Na is used2CO3Aid in synthesizing low silicon aluminum ratio X-type molecular sieve original powder
Under agitation successively by 2.488g sodium aluminates, 2.528g natrium carbonicum calcinatums, 2.979g solid sodium hydroxides,
2.847g solid potassium hydroxides are added in 19.9ml deionized waters and stirred to being completely dissolved, and are then slowly added into 3.64ml sodium metasilicate
Solution, 0.5h being stirred at room temperature, being eventually adding the directed agents for accounting for reactant gross mass 5%, room temperature condition continues lower stirring 1.0h；
By reactant at 60 DEG C static burn in 22h, the static crystallization 3h at 100 DEG C；After the completion of crystallization, slurry is separated into solid point
Son sieve and mother liquor, solid product are washed with water to neutrality, are dried at 100 DEG C, and product is produced after the completion of drying.
The mol ratio of each raw material is in step (2):SiO2/Al2O3=1.9, Na2O/(Na2O+K2O)=0.786, H2O/
SiO2=69, H2O/(Na2O+K2O)=13, Na2CO3/Na2O=0.3.
Embodiment 8：
One kind uses Na2CO3The method of synthesizing low silicon aluminum ratio X-type molecular sieve, specifically includes following steps：
(1) directed agents are prepared
By known technology, 1.382g sodium aluminate solids, 6.396g sodium hydroxides are added successively under agitation
In 18.6ml deionized waters, high alkalinity sodium aluminate solution is obtained, 6.4ml sodium silicate solutions are then slowly added to high alkalinity aluminic acid
In sodium solution, 0.5h is stirred at room temperature, it is directed agents to be stood under the conditions of 20 DEG C after aging 12h.
(2) Na is used2CO3Aid in synthesizing low silicon aluminum ratio X-type molecular sieve original powder
Under agitation successively by 2.488g sodium aluminates, 5.204g natrium carbonicum calcinatums, 0.040g solid sodium hydroxides,
2.306g solid potassium hydroxides are added in 19.6ml deionized waters and stirred to being completely dissolved, and are then slowly added into 4.0ml sodium metasilicate
Solution, 0.5h is stirred at room temperature, be eventually adding the directed agents for accounting for reactant gross mass 3%, continue to stir 0.5h under room temperature condition；
By reactant at 65 DEG C static burn in 15h, the static crystallization 4h at 100 DEG C；After the completion of crystallization, slurry is separated into solid point
Son sieve and mother liquor, solid product are washed with water to neutrality, are dried at 100 DEG C, and product is produced after the completion of drying.
The mol ratio of each raw material is in step (2):SiO2/Al2O3=2.1, Na2O/(Na2O+K2O)=0.8, H2O/SiO2
=62.5, H2O/(Na2O+K2O)=15, Na2CO3/Na2O=0.7.
Embodiment 9：
One kind uses Na2CO3The method of synthesizing low silicon aluminum ratio X-type molecular sieve, specifically includes following steps：
(1) directed agents are prepared
By known technology, 1.382g sodium aluminate solids, 6.396g sodium hydroxides are added successively under agitation
In 18.6ml deionized waters, high alkalinity sodium aluminate solution is obtained, 6.4ml sodium silicate solutions are then slowly added to high alkalinity aluminic acid
In sodium solution, 0.5h is stirred at room temperature, it is directed agents to be stood under the conditions of 30 DEG C after aging 8h.
(2) Na is used2CO3Aid in synthesizing low silicon aluminum ratio X-type molecular sieve original powder
Under agitation successively by 2.488g sodium aluminates, 3.532g natrium carbonicum calcinatums, 1.009g solid sodium hydroxides,
2.767g solid potassium hydroxides are added in 16.3ml deionized waters and stirred to being completely dissolved, and are then slowly added into 4.4ml sodium metasilicate
Solution, 0.5h is stirred at room temperature, be eventually adding the directed agents for accounting for reactant gross mass 4%, continue to stir 0.5h under room temperature condition；
By reactant at 60 DEG C static burn in 20h, the static crystallization 3.5h at 100 DEG C；After the completion of crystallization, slurry is separated into solid
Molecular sieve and mother liquor, solid product are washed with water to neutrality, are dried at 100 DEG C, and product is produced after the completion of drying.
The mol ratio of each raw material is in step (2):SiO2/Al2O3=2.3, Na2O/(Na2O+K2O)=0.76, H2O/
SiO2=50, H2O/(Na2O+K2O)=13.1, Na2CO3/Na2O=0.5.
The silica alumina ratio and relative crystallinity of the different instances synthetic sample of table 1
Note：XRD method n (SiO2/Al2O3) by empirical equation calculating gained：
a0 For the lattice constant of X-ray diffraction method determination sample.
Claims (5)
1. one kind uses Na2CO3The method for aiding in synthesizing low silicon aluminum ratio X-type molecular sieve, it is characterised in that comprise the following steps：
（1）Prepare directed agents：Silicon source and alkali source are first added to the water stirring to being completely dissolved to obtain high alkalinity sodium aluminate solution, so
Silicon source is slowly added into high alkalinity sodium aluminate solution afterwards, after stirring at room temperature, 15 DEG C ~ 30 DEG C 8 ~ 16h of static placement,
Produce required directed agents；The mol ratio of each raw material is Na wherein in directed agents2O:SiO2:Al2O3:H2O=17:5.76:1:250；
（2）Use Na2CO3Aid in synthesizing low silicon aluminum ratio X type molecular screen primary powders：
A, stock up
It is in molar ratio:SiO2/Al2O3=1.9~2.3,Na2O/(Na2O+K2O)=0.73~0.8, H2O/SiO2=50~69,H2O/
(Na2O+K2)=11 ~ 16, O wherein Na2CO3/Na2The ratio of O=0.3 ~ 0.7 feeds intake, measure respectively the silicon source of respective amount, silicon source,
Alkali source and water are as raw material；
B, plastic
Silicon source, alkali source and water are added in reactor successively under agitation, mixes to and is completely dissolved, then stirring
Add silicon source under state, 0.5 ~ 1h is stirred under room temperature condition, obtain mixture material, finally add 3% in mixture material ~
The directed agents of 5% mass percent, 0.5 ~ 1h is stirred at ambient temperature and carries out plastic；
C, aging and crystallization
After the completion of plastic, by mixture gel at 60 ~ 70 DEG C 8 ~ 22h of static burn in；After aging terminates, then by mixture gel
It is placed in 3 ~ 4h of static crystallization at 100 DEG C；
D, it is filtered, washed and dried
After the completion of crystallization, slurry is separated into solid molecular sieves and mother liquor, solid product is washed with water to neutrality, at 100 DEG C
Dry, produce using Na2CO3Aid in the low silica-alumina ratio X-type molecular sieve of synthesis.
2. one kind according to claim 1 uses Na2CO3The method for aiding in synthesizing low silicon aluminum ratio X-type molecular sieve, its feature
It is, step（1）In alkali source be solid sodium hydroxide or sodium hydrate aqueous solution.
3. one kind according to claim 2 uses Na2CO3The method for aiding in synthesizing low silicon aluminum ratio X-type molecular sieve, its feature
It is, described step（2）In alkali source be natrium carbonicum calcinatum, sodium hydroxide and potassium hydroxide solid mixture, either
Three's mixture solution.
4. one kind according to claim 2 uses Na2CO3The method for aiding in synthesizing low silicon aluminum ratio X-type molecular sieve, its feature
It is, step（1）With（2）In silicon source for sodium metasilicate or sodium metasilicate the aqueous solution.
5. one kind according to claim 2 uses Na2CO3The method for aiding in synthesizing low silicon aluminum ratio X-type molecular sieve, its feature
It is, step（1）With（2）In silicon source for sodium aluminate or sodium aluminate the aqueous solution.
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