CN108675314A - A kind of preparation method of lithium type low silicon aluminum than molecular sieve - Google Patents
A kind of preparation method of lithium type low silicon aluminum than molecular sieve Download PDFInfo
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- CN108675314A CN108675314A CN201810892367.7A CN201810892367A CN108675314A CN 108675314 A CN108675314 A CN 108675314A CN 201810892367 A CN201810892367 A CN 201810892367A CN 108675314 A CN108675314 A CN 108675314A
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
- C01B39/20—Faujasite type, e.g. type X or Y
- C01B39/22—Type X
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
- B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
- B01D53/047—Pressure swing adsorption
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
- B01J20/18—Synthetic zeolitic molecular sieves
- B01J20/186—Chemical treatments in view of modifying the properties of the sieve, e.g. increasing the stability or the activity, also decreasing the activity
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/10—Single element gases other than halogens
- B01D2257/102—Nitrogen
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Abstract
The present invention proposes a kind of lithium type low silicon aluminum than the preparation method of molecular sieve, includes the following steps：(1) synthesis of molecular sieve；(2) aging and crystallization；(3) washing and drying；(4) lithium ion exchanged；(5) prepared by type body.The present invention is exchanged by the liquid liquid of low silica-alumina ratio molecular sieve, it optimizes give-and-take conditions and obtains the adsorbent of high-lithium ion exchange, adsorption capacity than other domestic products is all high, is optimal adsorption and separation material in air separation process, is exclusively used in omnibus control system (VPSA) device.
Description
Technical field
A kind of preparation method the present invention relates to lithium type low silicon aluminum than molecular sieve.
Background technology
Lithium type low silicon aluminum ratio (Li-LSX types) molecular sieve is maximum to the adsorption capacity of nitrogen, nitrogen oxygen separating coefficient highest, and
Meet the absorption principle that pressure-variable adsorption High Pressure Absorption low pressure easily desorbs, is ideal pressure-variable adsorption nitrogen oxygen separating adsorbent.
Currently, domestic and foreign scholars are relatively fixed about LSX type Zeolite synthesis methods and each literature method is relatively more unified, base
This is hydro-thermal route；But, lithium ion exchanged step each document less for the document of lithium type low silicon aluminum ratio (Li-LSX) molecular sieve
Between be all different substantially, also have document refer to calcium ion, silver ion be modified, but document test be laboratory test, can not
Letter commercial performance test is judged.Domestic many producers have been able to production LSX molecular sieves, but can produce lithium type low silicon aluminum
Producer than (Li-LSX) molecular sieve is seldom, and lithium ion exchanged degree is at most merely able to reach 95%, leads to the lithium of external import
Type low silica-alumina ratio (Li-LSX) molecular sieve has monopolized domestic market, expensive.Meanwhile gradually pushing away with domestic PSA technology
Wide application, the country is to N2The demand of excellent lithium type low silicon aluminum ratio (Li-LSX) molecular sieve of absorption property will be very huge.Therefore,
Industrialized study of Li-LSX molecular sieves has long-range economic implications, however the lithium ion of existing general Li-LSX molecular sieves
Exchange rate be generally not more than 95%.
Invention content
The present invention proposes that a kind of lithium type low silicon aluminum than the preparation method of molecular sieve, can be made lithium ion exchanged rate and be higher than
95% adsorbent product, or even the lithium ion content of molecular sieve in adsorbent is made to reach total 99% or more of cation.
The technical proposal of the invention is realized in this way：
A kind of lithium type low silicon aluminum includes the following steps than the preparation method of molecular sieve：
Step 1, the synthesis of molecular sieve：A) by the sodium hydroxide solution of 25~35wt%, the potassium hydroxide of 40~45wt%
Solution is placed in round-bottomed flask and mixes, and is heated to 90 DEG C, stirring；B), in three times equivalent be added 15~20wt% aluminium hydroxide
Solution；C), 90 DEG C of heat preservation 4h；D) stop stirring, be cooled to room temperature；E) at room temperature by above-mentioned solution and deionized water in stainless steel
It is stirred in reaction kettle, is rapidly added 10~15wt% water glass solutions under high velocity agitation；
Step 2, aging and crystallization：Product aging at room temperature after the precipitation that step 1 is obtained, then at 80~95 DEG C
Lower crystallization；
Step 3, washing and drying：The precipitation that step 3 is obtained filters, and is first washed with NaOH solution, then use deionization
Water washing to filtrate pH value≤10, drying obtains LSX molecular sieves；
Step 4, lithium ion exchanged：A) the LiCl solution of 1.8~2.5mol/L is prepared；The urine of 1.0~1.5mol/L is added
Plain solution adjusts PH=8.0~8.5 by 25% ammonium hydroxide；B) pH=9.0~9.5 and then with LiOH by pH value are adjusted to；c)
It takes the LSX molecular screen primary powders that step 3 obtains to be added in LiCl solution, heats 50 DEG C, impregnate 2h, be then heated to 80 DEG C, 5h；
D) low speed centrifuge carries out precipitation separation, with NaOH solution alkali cleaning to pH=11.0~11.5；If e) repeating above-mentioned exchange process
Dry time to obtain satisfied ion-exchange degree；F) solid portion is dried in 80 DEG C of baking ovens；
It is prepared by step 5, type body：A) the Li-LSX molecular screen primary powders for obtaining step 5 and attapulgite are according to 2:1~4:
1 ratio is uniformly mixed；B) spherical shape that grain size is 0.7~0.8mm is made under certain rotating speed with sugar coating machine；C) it dries, roast
Industrial Li-LSX molecular sieve types body is made in sintering.
Preferably, in the step 1, the quality proportioning of reactant：Al2O3:Si02:NaK=1:(5.5~6.0):
(17.0~22.0).
Preferably, in the step 4, the reactant solid-liquid mass ratio in step c) is l:(10~15).
What the present invention generated has the beneficial effect that：The present invention prepares the lithium type low silicon aluminum for nitrogen oxygen separating than molecular sieve,
Difficult point prepared by product is lithium ion exchanged, liquid, the liquid that the present invention passes through solution and low silica-alumina ratio molecular sieve containing lithium ion
It exchanges, optimizes give-and-take conditions, obtain the adsorbent of high-lithium ion exchange, the adsorption capacity than other domestic products is all high, is
Optimal adsorption and separation material in air separation process.
Specific implementation mode
Technical scheme of the present invention is clearly and completely described below in conjunction with the embodiment of the present invention, it is clear that retouched
The embodiment stated is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, originally
The every other embodiment that field those of ordinary skill is obtained without making creative work, belongs to the present invention
The range of protection.
Embodiment 1：
Step 1, the synthesis of molecular sieve：A) by the sodium hydroxide solution of 25~35wt%, the potassium hydroxide of 40~45wt%
Solution is placed in round-bottomed flask and mixes, and is heated to 90 DEG C, stirring；B), in three times equivalent be added 15~20wt% aluminium hydroxide
Solution；C), 90 DEG C of heat preservation 4h；D) stop stirring, be cooled to room temperature；E) at room temperature by above-mentioned solution and deionized water in stainless steel
It is stirred in reaction kettle, is rapidly added 10~15wt% water glass solutions under high velocity agitation；The quality proportioning of reactant：
Al2O3:Si02:NaK=1:(5.5~6.0):(17.0~22.0)
Step 2, aging and crystallization：Product aging at room temperature after the precipitation that step 1 is obtained, then at 80~95 DEG C
Lower crystallization；
Step 3, washing and drying：The precipitation that step 3 is obtained filters, and is first washed with NaOH solution, then use deionization
Water washing to filtrate pH value≤10, drying obtains LSX molecular sieves；
Step 4, lithium ion exchanged：A) the LiCl solution of 1.8~2.5mol/L is prepared；The urine of 1.0~1.5mol/L is added
Plain solution adjusts PH=8.0 by 25% ammonium hydroxide；B) and then with LiOH by pH value it is adjusted to pH=9.5；C) step 3 is taken to obtain
To LSX molecular screen primary powders be added LiCl solution in, reactant solid-liquid mass ratio be l:(10~15) heat 50 DEG C, impregnate 2h,
80 DEG C are then heated to, 5h；D) low speed centrifuge carries out precipitation separation, with NaOH solution alkali cleaning to pH=11.0~11.5；e)
Above-mentioned exchange process is repeated several times to obtain satisfied ion-exchange degree；F) solid portion is dried in 80 DEG C of baking ovens；
It is prepared by step 5, type body：A) the Li-LSX molecular screen primary powders for obtaining step 5 and attapulgite are according to 2:1~4:
1 ratio is uniformly mixed；B) spherical shape that grain size is 0.7~0.8mm is made under certain rotating speed with sugar coating machine；C) it dries, roast
Industrial Li-LSX molecular sieve types body is made in sintering.
Embodiment 2：
Step 1, the synthesis of molecular sieve：A) by the sodium hydroxide solution of 25~35wt%, the potassium hydroxide of 40~45wt%
Solution is placed in round-bottomed flask and mixes, and is heated to 90 DEG C, stirring；B), in three times equivalent be added 15~20wt% aluminium hydroxide
Solution；C), 90 DEG C of heat preservation 4h；D) stop stirring, be cooled to room temperature；E) at room temperature by above-mentioned solution and deionized water in stainless steel
It is stirred in reaction kettle, is rapidly added 10~15wt% water glass solutions under high velocity agitation；The quality proportioning of reactant：
Al2O3:Si02:NaK=1:(5.5~6.0):(17.0~22.0)
Step 2, aging and crystallization：Product aging at room temperature after the precipitation that step 1 is obtained, then at 80~95 DEG C
Lower crystallization；
Step 3, washing and drying：The precipitation that step 3 is obtained filters, and is first washed with NaOH solution, then use deionization
Water washing to filtrate pH value≤10, drying obtains LSX molecular sieves；
Step 4, lithium ion exchanged：A) the LiCl solution of 1.8~2.5mol/L is prepared；The urine of 1.0~1.5mol/L is added
Plain solution adjusts PH=8.5 by 25% ammonium hydroxide；B) and then with LiOH by pH value it is adjusted to pH=9.0；C) step 3 is taken to obtain
To LSX molecular screen primary powders be added LiCl solution in, reactant solid-liquid mass ratio be l:(10~15) heat 50 DEG C, impregnate 2h,
80 DEG C are then heated to, 5h；D) low speed centrifuge carries out precipitation separation, with NaOH solution alkali cleaning to pH=11.0~11.5；e)
Above-mentioned exchange process is repeated several times to obtain satisfied ion-exchange degree；F) solid portion is dried in 80 DEG C of baking ovens；
It is prepared by step 5, type body：A) the Li-LSX molecular screen primary powders for obtaining step 5 and attapulgite are according to 2:1~4:
1 ratio is uniformly mixed；B) spherical shape that grain size is 0.7~0.8mm is made under certain rotating speed with sugar coating machine；C) it dries, roast
Industrial Li-LSX molecular sieve types body is made in sintering.
Comparative example 1：Using method same as Example 1, configuration LiCl solution is adjusted to identical using aluminium hydroxide
PH value, other are constant, finally be made industrial Li-LSX molecular sieve types body.
The finished product lithium type low silicon aluminum that embodiment 1-2, comparative example 1 are obtained carries out than molecular sieve (Li-LSX) and from city
Lithium ion in the molecular sieve bought on field is detected, and experimental result is as shown in table 1.
1 major parameter testing result of table
All there is apparent difference in the preparation method of the present invention and the prior art, while mainly by lithium ion exchanged
When, original powder is completed under heating stirring with the solution comprising lithium ion by ion-exchange process using liquid, liquid exchange process and is being improved
While lithium ion exchanged is spent, it is possible to reduce the usage amount of lithium salts can make the lithium ion content in molecular sieve reach cationic total
Several 99% or more.In addition, adjust pH value using urea and ammonium hydroxide in the present invention, change in the past using the substances such as aluminium hydroxide into
Row adjusts the mode of solution, and the substance wherein added is avoided to influence the constituent and catalytic performance of product, while the objects such as urea
Matter can improve the exchange degree of lithium ion in reaction while changing solution ph with slow release basic ion；And urea,
Ammonium hydroxide easily removes, and greatly improves the quality of product.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
With within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention god.
Claims (3)
1. a kind of lithium type low silicon aluminum is than the preparation method of molecular sieve, which is characterized in that include the following steps：
Step 1, the synthesis of molecular sieve：A) by the sodium hydroxide solution of 25~35wt%, the potassium hydroxide solution of 40~45wt%
It is placed in round-bottomed flask and mixes, be heated to 90 DEG C, stirring；B), in three times equivalent be added 15~20wt% aluminum hydroxide solution；
C), 90 DEG C of heat preservation 4h；D) stop stirring, be cooled to room temperature；E) at room temperature by above-mentioned solution and deionized water in stainless steel reaction
It is stirred in kettle, is rapidly added 10~15wt% water glass solutions under high velocity agitation；
Step 2, aging and crystallization：Product aging at room temperature after the precipitation that step 1 is obtained, then the crystalline substance at 80~95 DEG C
Change；
Step 3, washing and drying：The precipitation that step 3 is obtained filters, and is first washed with NaOH solution, then be washed with deionized water
It washs to filtrate pH value≤10, drying obtains LSX molecular sieves；
Step 4, lithium ion exchanged：A) the LiCl solution of 1.8~2.5mol/L is prepared；The urea that 1.0~1.5mol/L is added is molten
Liquid adjusts PH=8.0~8.5 by 25% ammonium hydroxide；B) pH=9.0~9.5 and then with LiOH by pH value are adjusted to；C) step is taken
Rapid three obtained LSX molecular screen primary powders are added in LiCl solution, heat 50 DEG C, impregnate 2h, be then heated to 80 DEG C, 5h；D) low
Fast centrifuge carries out precipitation separation, with NaOH solution alkali cleaning to pH=11.0~11.5；E) above-mentioned exchange process is repeated several times
To obtain satisfied ion-exchange degree；F) solid portion is dried in 80 DEG C of baking ovens；
It is prepared by step 5, type body：A) the Li-LSX molecular screen primary powders for obtaining step 5 and attapulgite are according to 2:1~4:1
Ratio is uniformly mixed；B) spherical shape that grain size is 0.7~0.8mm is made under certain rotating speed with sugar coating machine；C) it dries, roast and burn
Industrial Li-LSX molecular sieve types body is made in knot.
2. a kind of lithium type low silicon aluminum as described in claim 1 is than the preparation method of molecular sieve, which is characterized in that the step 1
In, the quality proportioning of reactant：Al2O3:Si02:NaK=1:(5.5~6.0):(17.0~22.0).
3. a kind of lithium type low silicon aluminum as described in claim 1 is than the preparation method of molecular sieve, which is characterized in that the step 4
In, the reactant solid-liquid mass ratio in step c) is l:(10~15).
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110743492A (en) * | 2019-10-18 | 2020-02-04 | 苏州立昂新材料有限公司 | Lithium type low silicon faujasite mixed with multivalent cations, method for preparing same and use thereof |
| CN113351157A (en) * | 2021-06-02 | 2021-09-07 | 昊华化工科技集团股份有限公司 | Modified lithium low-silicon zeolite molecular sieve and preparation method thereof |
| CN113979445A (en) * | 2021-11-29 | 2022-01-28 | 启东海奥华环保科技有限公司 | Lithium type low-silica-alumina ratio molecular sieve, preparation method and application thereof as adsorbent |
| CN114534436A (en) * | 2021-12-21 | 2022-05-27 | 南京瑞杨医用科技有限公司 | Medical molecular sieve oxygen generation system |
Citations (1)
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| CN102849754A (en) * | 2012-09-28 | 2013-01-02 | 上海恒业化工有限公司 | Ion exchange production method of molecular sieve |
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2018
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102849754A (en) * | 2012-09-28 | 2013-01-02 | 上海恒业化工有限公司 | Ion exchange production method of molecular sieve |
Non-Patent Citations (1)
| Title |
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| 林友文，石秀梅: "《全国普通高等医学院校五年制临床医学专业"十三五"规划教材 有机化学》", 31 August 2016 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110743492A (en) * | 2019-10-18 | 2020-02-04 | 苏州立昂新材料有限公司 | Lithium type low silicon faujasite mixed with multivalent cations, method for preparing same and use thereof |
| CN113351157A (en) * | 2021-06-02 | 2021-09-07 | 昊华化工科技集团股份有限公司 | Modified lithium low-silicon zeolite molecular sieve and preparation method thereof |
| CN113979445A (en) * | 2021-11-29 | 2022-01-28 | 启东海奥华环保科技有限公司 | Lithium type low-silica-alumina ratio molecular sieve, preparation method and application thereof as adsorbent |
| CN114534436A (en) * | 2021-12-21 | 2022-05-27 | 南京瑞杨医用科技有限公司 | Medical molecular sieve oxygen generation system |
| CN114534436B (en) * | 2021-12-21 | 2023-03-10 | 南京瑞杨医用科技有限公司 | Medical molecular sieve oxygen generation system |
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Application publication date: 20181019 |