CN106892438A - A kind of preparation method of 4A zeolites - Google Patents
A kind of preparation method of 4A zeolites Download PDFInfo
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- CN106892438A CN106892438A CN201710073876.2A CN201710073876A CN106892438A CN 106892438 A CN106892438 A CN 106892438A CN 201710073876 A CN201710073876 A CN 201710073876A CN 106892438 A CN106892438 A CN 106892438A
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- zeolites
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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
- C01B39/16—Type A from aqueous solutions of an alkali metal aluminate and an alkali metal silicate excluding any other source of alumina or silica but seeds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/11—Powder tap density
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/90—Other properties not specified above
Abstract
The invention discloses a kind of preparation method of 4A zeolites.Sodium aluminate solution and sodium silicate solution carry out pulp reaction, then add 4A zeolites as crystal seed, and after stirring, intensification crystallization, you can good to obtain absorption property, tap density is more than 0.8g/cm34A zeolite products.Invention not only simplifies technological process prepared by traditional 4A zeolites, without preparing new crystal seed, 4A zeolite preparation costs are greatly reduced, and products obtained therefrom adsorption capacity is high, and tap density is big, has broad application prospects in molecular sieve industry.
Description
Technical field
The present invention relates to zeolite preparing technical field, more particularly to a kind of preparation method of 4A zeolites.
Background technology
4A zeolites are widely used in washing assisant, absorption, plastics at present as a kind of zeolite product of excellent performance
The industries such as stabilizer.Since the nineties in last century, 4A zeolites manufacturing enterprise sets up successively, sustainable development.The production of 4A zeolites
Method has a lot, wherein commonplace with hydrothermal synthesis method.Its raw material is in addition to sodium metasilicate, and the preparation method of sodium aluminate is each not
It is identical.Have with aluminium hydroxide as raw material, prepare sodium aluminate with NaOH dissolving；Have with the mining hydroxide of import alum clay
Sodium dissolving prepares sodium aluminate；What is had directly prepares 4A zeolites with the sodium aluminate solution in alumina by sintering production process；It is near several
Year, there are many enterprises directly directly to be reacted with sodium metasilicate with the aluminium hydroxide decomposition nut liquid of Bayer process alumina producing and prepare 4A boilings
Stone.In earliest 4A zeolite production processes, without directed agents, high temperature crystallization is not only needed, and crystallization time is long, it is final to produce
Product index is also poor.After 2000, each 4A zeolites manufacturing enterprise reduces production cost for improve product quality, all starts
Addition directed agents are as crystal seed so that product quality is enhanced.
Directing agent method produces 4A zeolites, although can reduce production cost, improve product quality, but the product for being produced
Granularity is thinner, and tap density is smaller.The 4A zeolite products of method production are relatively specific for washing assisant and stabilizer for plastics industry.
And the adsorbent industry to there is particular/special requirement, for especially requiring the adsorbent of high-tap density, using directing agent method with regard to nothing
Method meets its requirement.Therefore, research one kind can reduce 4A zeolite production costs, and the 4A zeolites of its tap density can be improved again
Preparation method meet the application that special binding molecule sieves industry, be of great significance.
The content of the invention
The present invention provides a kind of preparation method of 4A zeolites aiming at above-mentioned defect, there is provided one kind prepares height
Adsorptivity, while the 4A zeolites of high-tap density, simple to operate, quality is steady during 4A zeolite product preparation process can be ensured again
Fixed new method.
A kind of preparation method technical scheme of 4A zeolites of the invention is that sodium aluminate solution and sodium silicate solution carry out pulp
Reaction, then adds 4A zeolites as crystal seed, after stirring, intensification crystallization, you can good to obtain absorption property, tap density is more than
0.8g/cm34A zeolite products.
A kind of preparation method of described 4A zeolites, processing step includes successively：
(1) by sodium aluminate solution and sodium silicate solution, by SiO2/Al2O3Mol ratio be 2.0, under the conditions of 45-60 DEG C
Mixing carries out pulp reaction；
(2) add 4A zeolites as crystal seed, continue to stir；
(3) intensification carries out crystallization and obtains crystallization liquid；
(4) crystallization liquid filtered, washed, dried, that is, it is good to obtain absorption property, tap density is more than 0.8g/cm3's
4A zeolite products.
In step (1), the Al of sodium aluminate solution2O3Concentration is 50-100g/L, and Crater corrosion is 1.8-2.5；Sodium silicate solution
SiO2Concentration is 150-240g/L, and modulus is 3.0.
In step (2), after pulp reaction 0.5-1h, addition 4A zeolites continue to stir 0.5h as crystal seed.
In step (2), seed load is 2-5g/L, and cumulative volume is with pulp liquid stereometer.
In step (2), as the 4A zeolites that crystal seed is added, its granularity D50 is 1-3 μm.
In step (3), 75-100 DEG C is warming up to.
In step (3), the crystallization time is 2-4h.
In step (4), resulting 4A zeolite products, Static Water adsorbs more than 26.5mg/g.
Beneficial effects of the present invention are：The method of the present invention be in 4A zeolite production processes, with 4A zeolites in itself as
Crystal seed, not only shortens the reaction time, and without preparing 4A zeolite seed crystals in addition, it is simple to operate, reduce production cost.
Instant invention overcomes in existing 4A zeolite preparing process, the shortcoming that temperature is high, the time is long it also avoid directing agent method
The shortcoming of the small 4A zeolites of fine size, tap density can only be produced.On the basis of same reduction production cost, can prepare and shake
Real density 4A zeolite products high, the development to molecular sieve adsorption industry will bring profound significance.
Specific embodiment：
For a better understanding of the present invention, technical scheme is described in detail with instantiation below, but originally
Invention is not limited thereto.
Embodiment 1
(1) it is 2.1, Al by Crater corrosion2O3Concentration is the sodium aluminate solution of 65g/L, is that 3.0, SiO2 concentration is with modulus
The sodium silicate solution of 210g/L, according to a mole SiO2/Al2O3It is 2.0 ratio, is mixed under the conditions of 50 DEG C, carries out pulp
Reaction.
(2) after pulp reaction 0.5h, according to pulp volume, the 4A zeolites of 3g/L, the 4A boilings of addition are added toward pulp liquid
Stone granularity D50 is 2.1 μm, continues to stir 0.5h.
(3) pulp liquid temperature degree is brought up to 75 DEG C with steam, carries out crystallization.
(4) after crystallization 3h, that is, qualified 4A zeolite slurries are obtained.
(5) by 4A zeolites slurry by filtering, washing, drying, the 4A zeolite product Static Waters for obtaining are adsorbed as 26.8mg/
G, granularity D50 are 5.4 μm, and tap density is 0.83g/cm3。
Embodiment 2
(1) it is 1.9, Al by Crater corrosion2O3Concentration is the sodium aluminate solution of 76g/L, is that 3.0, SiO2 concentration is with modulus
The sodium silicate solution of 180g/L, according to a mole SiO2/Al2O3It is 2.0 ratio, is mixed under the conditions of 55 DEG C, carries out pulp
Reaction.
(2) after pulp reaction 1h, according to pulp volume, the 4A zeolites of 2.5g/L, the 4A boilings of addition are added toward pulp liquid
Stone granularity D50 is 2.5 μm, continues to stir 0.5h.
(3) pulp liquid temperature degree is brought up to 80 DEG C with steam, carries out crystallization.
(4) after crystallization 3h, that is, qualified 4A zeolite slurries are obtained.
(5) by 4A zeolites slurry by filtering, washing, drying, the 4A zeolite product Static Waters for obtaining are adsorbed as 27.1mg/
G, granularity D50 are 5.7 μm, and tap density is 0.85g/cm3。
Embodiment 3
(1) it is 2.5, Al by Crater corrosion2O3Concentration is the sodium aluminate solution of 70g/L, is that 3.0, SiO2 concentration is with modulus
The sodium silicate solution of 240g/L, according to a mole SiO2/Al2O3It is 2.0 ratio, is mixed under the conditions of 55 DEG C, carries out pulp
Reaction.
(2) after pulp reaction 0.5h, according to pulp volume, the 4A zeolites of 3.5g/L, the 4A of addition are added toward pulp liquid
Zeolite particle size D50 is 3.0 μm, continues to stir 0.5h.
(3) pulp liquid temperature degree is brought up to 75 DEG C with steam, carries out crystallization.
(4) after crystallization 2.5h, that is, qualified 4A zeolite slurries are obtained.
(5) by 4A zeolites slurry by filtering, washing, drying, the 4A zeolite product Static Waters for obtaining are adsorbed as 26.9mg/
G, granularity D50 are 5.4 μm, and tap density is 0.84g/cm3。
Embodiment 4
(1) it is 1.9, Al by Crater corrosion2O3Concentration is the sodium aluminate solution of 55g/L, is 3.0, SiO with modulus2Concentration is
The sodium silicate solution of 150g/L, according to a mole SiO2/Al2O3It is 2.0 ratio, is mixed under the conditions of 55 DEG C, carries out pulp
Reaction.
(2) after pulp reaction 1h, according to pulp volume, the 4A zeolites of 4g/L, the 4A zeolites of addition are added toward pulp liquid
Granularity D50 is 3.0 μm, continues to stir 0.5h.
(3) pulp liquid temperature degree is brought up to 85 DEG C with steam, carries out crystallization.
(4) after crystallization 3h, that is, qualified 4A zeolite slurries are obtained.
(5) by 4A zeolites slurry by filtering, washing, drying, the 4A zeolite product Static Waters for obtaining are adsorbed as 27.2mg/
G, granularity D50 are 5.9 μm, and tap density is 0.88g/cm3。
Embodiment 5
(1) it is 2.4, Al by Crater corrosion2O3Concentration is the sodium aluminate solution of 85g/L, is 3.0, SiO with modulus2Concentration is
The sodium silicate solution of 180g/L, according to a mole SiO2/Al2O3It is 2.0 ratio, is mixed under the conditions of 60 DEG C, carries out pulp
Reaction.
(2) after pulp reaction 0.5h, according to pulp volume, the 4A zeolites of 3.5g/L, the 4A of addition are added toward pulp liquid
Zeolite particle size D50 is 3.0 μm, continues to stir 0.5h.
(3) pulp liquid temperature degree is brought up to 80 DEG C with steam, carries out crystallization.
(4) after crystallization 3h, that is, qualified 4A zeolite slurries are obtained.
(5) by 4A zeolites slurry by filtering, washing, drying, the 4A zeolite product Static Waters for obtaining are adsorbed as 26.9mg/
G, granularity D50 are 5.1 μm, and tap density is 0.81g/cm3。
Embodiment 6
(1) it is 1.8, Al by Crater corrosion2O3Concentration is the sodium aluminate solution of 85g/L, is 3.0, SiO with modulus2Concentration is
The sodium silicate solution of 240g/L, according to a mole SiO2/Al2O3It is 2.0 ratio, is mixed under the conditions of 45 DEG C, carries out pulp
Reaction.
(2) after pulp reaction 0.5h, according to pulp volume, the 4A zeolites of 4g/L, the 4A boilings of addition are added toward pulp liquid
Stone granularity D50 is 2.4 μm, continues to stir 0.5h.
(3) pulp liquid temperature degree is brought up to 85 DEG C with steam, carries out crystallization.
(4) after crystallization 2h, that is, qualified 4A zeolite slurries are obtained.
(5) by 4A zeolites slurry by filtering, washing, drying, the 4A zeolite product Static Waters for obtaining are adsorbed as 26.7mg/
G, granularity D50 are 6.1 μm, and tap density is 0.92g/cm3。
Claims (9)
1. a kind of preparation method of 4A zeolites, it is characterised in that sodium aluminate solution and sodium silicate solution carry out pulp reaction, then
As crystal seed, after stirring, intensification crystallization, you can good to obtain absorption property, tap density is more than 0.8g/cm to addition 4A zeolites3
4A zeolite products.
2. the preparation method of a kind of 4A zeolites according to claim 1, it is characterised in that processing step includes successively：
(1) by sodium aluminate solution and sodium silicate solution, by SiO2/Al2O3Mol ratio be 2.0, under the conditions of 45-60 DEG C mix
Stirring carries out pulp reaction；
(2) add 4A zeolites as crystal seed, continue to stir；
(3) intensification carries out crystallization and obtains crystallization liquid；
(4) crystallization liquid filtered, washed, dried, that is, it is good to obtain absorption property, tap density is more than 0.8g/cm34A boiling
Stone product.
3. the preparation method of a kind of 4A zeolites according to claim 1, it is characterised in that in step (1), sodium aluminate solution
Al2O3Concentration is 50-100g/L, and Crater corrosion is 1.8-2.5；Sodium silicate solution SiO2Concentration is 150-240g/L, and modulus is
3.0。
4. the preparation method of a kind of 4A zeolites according to claim 1, it is characterised in that in step (2), pulp reaction
After 0.5-1h, addition 4A zeolites continue to stir 0.5h as crystal seed.
5. the preparation method of a kind of 4A zeolites according to claim 1, it is characterised in that in step (2), seed load
It is 2-5g/L.
6. the preparation method of a kind of 4A zeolites according to claim 1, it is characterised in that in step (2), as crystal seed institute
The 4A zeolites of addition, its granularity D50 is 1-3 μm.
7. the preparation method of a kind of 4A zeolites according to claim 1, it is characterised in that in step (3), be warming up to 75-
100℃。
8. the preparation method of a kind of 4A zeolites according to claim 1, it is characterised in that in step (3), during crystallization
Between be 2-4h.
9. the preparation method of a kind of 4A zeolites according to claim 1, it is characterised in that in step (4), resulting 4A
Zeolite product, Static Water adsorbs more than 26.5mg/g.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108128783A (en) * | 2018-03-15 | 2018-06-08 | 山东鲁北企业集团总公司 | A kind of preparation method of 3A zeolite molecular sieves original powder |
| CN112218711A (en) * | 2018-06-05 | 2021-01-12 | 东洋纺株式会社 | Adsorption sheet, method for producing adsorption sheet, and adsorption element |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1454842A (en) * | 2002-04-30 | 2003-11-12 | 上海信渊实业有限公司 | 4A zeolite, manufacture method and use thereof |
| CN101337680A (en) * | 2008-08-07 | 2009-01-07 | 中国科学院新疆理化技术研究所 | Method for synthesizing 4A zeolite molecular sieve by adding guiding agent |
| CN101693542A (en) * | 2009-10-09 | 2010-04-14 | 西安建筑科技大学 | Production method of 4-A molecular sieve |
| CN105197957A (en) * | 2015-10-15 | 2015-12-30 | 内蒙古日盛可再生资源有限公司 | Synthetic method of zeolite 4A |
| CN106276959A (en) * | 2016-08-16 | 2017-01-04 | 中国铝业股份有限公司 | Spherical 4A zeolite, its preparation method, preparation facilities and purposes |
-
2017
- 2017-02-10 CN CN201710073876.2A patent/CN106892438A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1454842A (en) * | 2002-04-30 | 2003-11-12 | 上海信渊实业有限公司 | 4A zeolite, manufacture method and use thereof |
| CN101337680A (en) * | 2008-08-07 | 2009-01-07 | 中国科学院新疆理化技术研究所 | Method for synthesizing 4A zeolite molecular sieve by adding guiding agent |
| CN101693542A (en) * | 2009-10-09 | 2010-04-14 | 西安建筑科技大学 | Production method of 4-A molecular sieve |
| CN105197957A (en) * | 2015-10-15 | 2015-12-30 | 内蒙古日盛可再生资源有限公司 | Synthetic method of zeolite 4A |
| CN106276959A (en) * | 2016-08-16 | 2017-01-04 | 中国铝业股份有限公司 | Spherical 4A zeolite, its preparation method, preparation facilities and purposes |
Non-Patent Citations (1)
| Title |
|---|
| 汪多仁: "《绿色净水处理剂》", 30 November 2006 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108128783A (en) * | 2018-03-15 | 2018-06-08 | 山东鲁北企业集团总公司 | A kind of preparation method of 3A zeolite molecular sieves original powder |
| CN108128783B (en) * | 2018-03-15 | 2021-04-09 | 山东鲁北企业集团总公司 | Preparation method of 3A zeolite molecular sieve raw powder |
| CN112218711A (en) * | 2018-06-05 | 2021-01-12 | 东洋纺株式会社 | Adsorption sheet, method for producing adsorption sheet, and adsorption element |
| CN112218711B (en) * | 2018-06-05 | 2024-04-05 | 东洋纺Mc株式会社 | Adsorption sheet, method for producing adsorption sheet, and adsorption element |
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