CN106365176A - Preparation method of 3A molecular sieve - Google Patents
Preparation method of 3A molecular sieve Download PDFInfo
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- CN106365176A CN106365176A CN201610741722.1A CN201610741722A CN106365176A CN 106365176 A CN106365176 A CN 106365176A CN 201610741722 A CN201610741722 A CN 201610741722A CN 106365176 A CN106365176 A CN 106365176A
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- exchange
- molecular sieve
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- filter pressing
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- 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
- C01B39/14—Type A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B01J20/16—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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Analytical Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention provides a preparation method of a 3A molecular sieve. The preparation method includes the steps of primary exchange and secondary exchange. Primary exchange includes the following steps that a 4A molecular sieve and potassium-containing washing water recycled through secondary exchange are mixed and stirred in a primary exchange tank for exchange, filter-press washing is carried out after exchange is completed, and a primary filter-press material is obtained. Secondary exchange includes the following steps that the primary filter-press material, water and potassium chloride are mixed and stirred in a secondary exchange tank for exchange, press-filter washing is carried out after exchange is completed, and a secondary press-filter material and potassium-containing washing water are obtained, the potassium-containing washing water is recycled into primary exchange to participate in exchange, and after the secondary press-filter material is subjected to press-filter washing with water, the 3A molecular sieve is prepared through drying.
Description
Technical field
The present invention relates to a kind of preparation method of 3a molecular sieve.
Background technology
Chinese patent literature cn102351213a discloses a kind of method preparing 3a type zeolite molecular sieve, walks including following
Rapid: 1), kaolinic calcining: Lincang soft kaolin to be calcined 3-5 hour at 550-700 DEG C, obtains metakaolin；2)、
The preparation of 4a molecular sieve: the proportioning by metakaolin and naoh aqueous solution is: 1530g:100ml, chooses metakaolin and naoh
Aqueous solution, wherein, the concentration of naoh aqueous solution is 2-5mol/l；By metakaolin with naoh aqueous solution uniformly, it is warming up to
60-80 DEG C, strong stirring effect lower ageing 3-5 hour, then it is warmed up to 90-100 DEG C, moderate-speed mixer 4-6 hour, obtain mixture；
Mixture is filtered, filter cake filters after distilled water wash again, filtering gained filter cake again, 2-4 to be dried in 90-100 DEG C little
When, obtain 4a molecular sieve；3), the preparation of 3a type zeolite molecular sieve: the proportioning by 4a molecular sieve and kcl solution is: 5-10g:
100ml, chooses 4a molecular sieve and kcl solution, and wherein, the concentration of kcl solution is 2-5mol/l；By 4a molecular sieve and kcl solution
Under the conditions of 70-90 DEG C, in a kettle. react 3-5 hour, more cooled, washing, filter, filter gained filter cake in 90-100
2-4 hour DEG C is dried, obtains 3a type zeolite molecular sieve；In the preparation technology of above-mentioned 3a molecular sieve, k ion cannot completely and 4a
Na ion exchange in molecular sieve, k ionic availability is low, and k ion is low with the exchange rate of na ion, and after filtration washing, containing k
The wash water of ion will be drained off, and pollutes environment.
In addition, typically between 38-55%, relative water adsorptive value is in 25-23.5% for the exchange rate of existing 3a molecular sieve
Between, and exchange rate is higher, water adsorptive value is lower, and this is a big defect, and technical barrier therein is to improve k ion
Replace more na ions, after more k ionic replacement na ion, more adsorption holes can be blocked again, lead to water adsorptive value
Low.
Content of the invention
The purpose of the present invention is for the deficiencies in the prior art, provide one kind can effectively utilizes k ion, the 3a of energy-saving and emission-reduction
Molecular sieve preparation method, the ion exchange ratio of prepared 3a molecular sieve is high, and has good water absorption.
The purpose of the present invention to be realized by following technical solution:
A kind of preparation method of 3a molecular sieve it is characterised in that: include once exchange and secondary exchange,
Once exchange and comprise the steps: 4a molecular sieve and the secondary wash water containing potassium reclaiming that exchanges in a swap tank
Mix and blend swaps, and after the completion of exchange, pressure filtration washing obtains a filter pressing material；
Secondary exchange comprises the steps: to enter filter pressing material, water and potassium chloride mix and blend in secondary swap tank
Row exchanges, and after the completion of exchange, pressure filtration washing obtains secondary filter pressing material and wash water containing potassium, will contain potassium wash water and be recycled in once exchange
Participate in exchanging, by secondary filter pressing material with, after hydraulic pressure filter washing, drying and 3a molecular sieve being obtained.
Further, fed intake by solid-liquid mass ratio 1:4 in a swap tank.
Further, fed intake by solid-liquid mass ratio 1:4 in secondary swap tank, wherein, a filter pressing material and chlorination
The mass ratio of potassium is 0.26:1.
Further, the described exchange temperature once exchanging is 60-80 DEG C, and swap time is 25-40 minute.
Further, the exchange temperature of described secondary exchange is 60-80 DEG C, and swap time is 25-40 minute.
Further, first water is put in secondary swap tank in described secondary exchange, then put into potassium chloride, potassium to be chlorinated
Put into a filter pressing material after being completely dissolved, after stirring, be warming up to exchange temperature.
The invention has the following beneficial effects:
The 3a molecular sieve preparation method that present invention offer exchanges twice, washing containing potassium using secondary exchange in once exchanging
Water is swapped with 4a molecular sieve, is carried out with Klorvess Liquid using once exchanging the filter pressing material obtaining in secondary exchange
Exchanging, and potassium wash water will be contained and be recycled in once exchange, thus constituting recycling of potassium ion, reducing potassium chloride dosage, and
Exchange twice and can improve ion exchange ratio again, and the dissolution time of potassium can be reduced, greatly shorten the production time, in addition one
In the wash water that the pressure filtration washing of secondary exchange is discharged, the content of potassium is few, mainly contains sodium ion and chloride ion, is expelled directly out to environment
Pollution little.
Brief description
Below in conjunction with the accompanying drawings the present invention is described in further detail.
Fig. 1 is the process chart of the present invention.
Specific embodiment
Embodiment one, with reference to shown in Fig. 1, a kind of preparation method of 3a molecular sieve, including once exchange and secondary exchange.
Once exchange and comprise the steps: 4a molecular sieve (na2o·al2o3·2sio29/2h2o) with secondary exchange
The wash water containing potassium reclaiming presses solid-liquid mass ratio 1:4 mixing and stirring in a swap tank, then heats to 80 DEG C, dynamically stirs
Mix exchange 30 minutes, after the completion of exchange, pressure filtration washing obtains a filter pressing material and containing sodium ion, chloride ion and a small amount of potassium ion
Wash water, wash water is carried out waste discharge process, and a filter pressing material is sent in secondary exchange；
Secondary exchange comprises the steps: first to put into water in secondary swap tank, then puts into potassium chloride, and potassium to be chlorinated is complete
Put into a filter pressing material after dissolving, after stirring, be warming up to 75 DEG C, dynamic agitation exchanges 30 minutes, pressure filtering cleaning after the completion of exchange
Wash and obtain secondary filter pressing material and wash water containing potassium, wash water containing potassium is recycled in once exchanging and participates in exchanging, and secondary filter pressing material is used certainly again
Water filtration washing, is carried out by solid-liquid mass ratio 1:4 in secondary swap tank to ph≤11, then drying to 3a molecular sieve
Feed intake, wherein, the mass ratio of a filter pressing material and potassium chloride is 0.26:1.
Embodiment two, with reference to shown in Fig. 1, a kind of preparation method of 3a molecular sieve, including once exchange and secondary exchange.
Once exchange and comprise the steps: 4a molecular sieve (na2o·al2o3·2sio29/2h2o) with secondary exchange
The wash water containing potassium reclaiming presses solid-liquid mass ratio 1:4 mixing and stirring in a swap tank, then heats to 75 DEG C, dynamically stirs
Mix exchange 30 minutes, after the completion of exchange, pressure filtration washing obtains a filter pressing material and containing sodium ion, chloride ion and a small amount of potassium ion
Wash water, wash water is carried out waste discharge process, and a filter pressing material is sent in secondary exchange；
Secondary exchange comprises the steps: first to put into water in secondary swap tank, then puts into potassium chloride, and potassium to be chlorinated is complete
Put into a filter pressing material after dissolving, after stirring, be warming up to 75 DEG C, dynamic agitation exchanges 30 minutes, pressure filtering cleaning after the completion of exchange
Wash and obtain secondary filter pressing material and wash water containing potassium, wash water containing potassium is recycled in once exchanging and participates in exchanging, and secondary filter pressing material is used certainly again
Water filtration washing, is carried out by solid-liquid mass ratio 1:4 in secondary swap tank to ph≤11, then drying to 3a molecular sieve
Feed intake, wherein, the mass ratio of a filter pressing material and potassium chloride is 0.26:1.
Following performance is had using the 3a molecular sieve that above-mentioned technique is obtained:
| Embodiment one | Embodiment two | Existing product 1 | Existing product 1 | Existing product 1 | |
| Static Water is adsorbed | 24.75% | 24.73% | 24.45% | 24.60% | 24.67% |
| Exchange rate | 58% | 59% | 50% | 45% | 45% |
The above, only presently preferred embodiments of the present invention, therefore the scope that the present invention is implemented can not be limited with this, that is,
The equivalence changes made according to scope of the present invention patent and description and modification, all should still belong to what patent of the present invention covered
In the range of.
Claims (6)
1. a kind of preparation method of 3a molecular sieve it is characterised in that: include once exchange and secondary exchange,
Once exchange and comprise the steps: to mix 4a molecular sieve in a swap tank with the secondary wash water containing potassium reclaiming that exchanges
Stirring swaps, and after the completion of exchange, pressure filtration washing obtains a filter pressing material；
Secondary exchange comprises the steps: to be handed over filter pressing material, water and potassium chloride mix and blend in secondary swap tank
Change, after the completion of exchange, pressure filtration washing obtains secondary filter pressing material and wash water containing potassium, potassium wash water will be contained and be recycled to participation in once exchange
Exchange, by secondary filter pressing material with, after hydraulic pressure filter washing, drying and 3a molecular sieve being obtained.
2. a kind of 3a molecular sieve according to claim 1 preparation method it is characterised in that: press solid in a swap tank
Liquid mass ratio 1:4 is fed intake.
3. a kind of 3a molecular sieve according to claim 1 preparation method it is characterised in that: press solid in secondary swap tank
Liquid mass ratio 1:4 is fed intake, and wherein, the mass ratio of a filter pressing material and potassium chloride is 0.26:1.
4. a kind of 3a molecular sieve according to claim 1 or 2 or 3 preparation method it is characterised in that: described once exchange
Exchange temperature be 60-80 DEG C, swap time be 25-40 minute.
5. a kind of 3a molecular sieve according to claim 1 or 2 or 3 preparation method it is characterised in that: described secondary exchange
Exchange temperature be 60-80 DEG C, swap time be 25-40 minute.
6. a kind of 3a molecular sieve according to claim 1 or 2 or 3 preparation method it is characterised in that: in described secondary friendship
Change and first put into water in secondary swap tank, then put into potassium chloride, potassium to be chlorinated puts into a filter pressing material, stirring after being completely dissolved
It is warming up to exchange temperature after uniformly.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610741722.1A CN106365176A (en) | 2016-08-26 | 2016-08-26 | Preparation method of 3A molecular sieve |
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| CN201610741722.1A CN106365176A (en) | 2016-08-26 | 2016-08-26 | Preparation method of 3A molecular sieve |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107720772A (en) * | 2017-09-26 | 2018-02-23 | 郑州雪山实业股份有限公司 | Special 3A G activation powder of double glazing adhesive tape and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1248487A (en) * | 1998-09-24 | 2000-03-29 | 广州经济技术开发区商业服务总公司 | Secondary perforated molecular siever adsorbent and preparation process thereof |
| CN102351213A (en) * | 2011-07-21 | 2012-02-15 | 中国地质大学（武汉） | Method for preparing 3A type zeolite molecular sieve |
| 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 |
| CN103721673A (en) * | 2014-01-06 | 2014-04-16 | 郑州富龙新材料科技有限公司 | Preparation method of K-A molecular sieve |
| CN105800638A (en) * | 2012-04-16 | 2016-07-27 | 山东能特异能源科技有限公司 | Low-potassium type 3A zeolite molecular sieve and preparation method thereof |
-
2016
- 2016-08-26 CN CN201610741722.1A patent/CN106365176A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1248487A (en) * | 1998-09-24 | 2000-03-29 | 广州经济技术开发区商业服务总公司 | Secondary perforated molecular siever adsorbent and preparation process thereof |
| CN102351213A (en) * | 2011-07-21 | 2012-02-15 | 中国地质大学（武汉） | Method for preparing 3A type zeolite molecular sieve |
| CN105800638A (en) * | 2012-04-16 | 2016-07-27 | 山东能特异能源科技有限公司 | Low-potassium type 3A zeolite molecular sieve and preparation method thereof |
| 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 |
| CN103721673A (en) * | 2014-01-06 | 2014-04-16 | 郑州富龙新材料科技有限公司 | Preparation method of K-A molecular sieve |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107720772A (en) * | 2017-09-26 | 2018-02-23 | 郑州雪山实业股份有限公司 | Special 3A G activation powder of double glazing adhesive tape and preparation method thereof |
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