CN1213945C - Technological process and special apparatus for preparing 4A zeolite - Google Patents
Technological process and special apparatus for preparing 4A zeolite Download PDFInfo
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- CN1213945C CN1213945C CN 03122335 CN03122335A CN1213945C CN 1213945 C CN1213945 C CN 1213945C CN 03122335 CN03122335 CN 03122335 CN 03122335 A CN03122335 A CN 03122335A CN 1213945 C CN1213945 C CN 1213945C
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Abstract
The present invention relates to a technology for preparing 4A zeolite. Silicon sources are dissolved in water or an alkali solution to be prepared into a sodium silicate solution; aluminum sources are dissolved in an alkali solution to be prepared into a sodium aluminate solution; the sodium silicate solution and the sodium aluminate solution respectively and continuously enter a reaction vessel through pipelines; subsequently, the sodium silicate solution and the sodium aluminate solution enter a crystallization vessel for crystallization, filtration, washing, drying and forming powder to obtain 4A zeolite productsr. The present invention has the advantages of simplicity, easy implementation, small device, low cost and high repeatability. The synthesized 4A zeolite has the advantages of narrow particle size distribution, perfect crystal form and high crystallinity, and can be used for continuous production.
Description
Technical field:
The present invention is the synthetic method that belongs to a kind of 4A zeolite, relates in particular to a kind of synthesis technique and specific equipment thereof of 4A zeolite.
Background technology:
The synthetic method of 4A zeolite mainly is a rhythmic reaction under the stirring of stirring tank, adopts the reinforced method of turbulent flow and two sections synthetic 4A zeolites of crystallization process synchronously as report in the Chinese patent 1017160 (notification number); Report is by the synthetic 4A zeolite of the technology of mixing back crystallization in crystallizing kettle in pipeline in the United States Patent (USP) 0010034067; Report is adopted the synthetic 4A zeolite of two-step process in the United States Patent (USP) 4469036; Two-step process synthetic zeolite Akira Yoshida etc. is zeolite magazine 1991 in addition, described the technology of the synthetic 4A zeolite of two-step approach 11 volumes, 94 pages of " preparing the 4A zeolite from water glass " literary compositions.Do not appear in the newspapers as yet from the serialization production of the raw material whole technology of product to the end.
Summary of the invention:
The present invention provides a kind of continuous process and specific equipment thereof of synthetic 4A zeolite.
The present invention is achieved in that certain density sodium silicate solution and the sodium aluminate solution mixing pump by reacts gel, the gel product crystallization that in specific equipment, heats up, then crystallization product carries out washing and filtering on the filtration unit of a serialization, and final drying gets high-quality 4A zeolite.
Synthetic method of the present invention comprises the steps:
The silicon source is configured to Na in the water-soluble or alkali lye
2O content is 45-105g/l; SiO
2Content is the sodium silicate solution of 120-350g/l; The aluminium source is dissolved in and is configured to Na in the alkali lye
2O content is 70-120g/l; Al
2O
3Content is the sodium aluminate solution of 40-70g/l;
Above-mentioned two kinds of solution are 1-6 by silica alumina ratio, enter mixing reactor continuously by pipeline respectively and carry out the hybrid reaction gel, then entering the crystallization device is 60-100 ℃ in temperature, and flow velocity is 0.1-10m/min, and the residence time is to carry out crystallization under the condition of 10-60min;
By continuous filtration, remove mother liquor after the crystallization, and utilize the deionized water wash pH value to 7-11, the mother liquor under filtering is back to use in the preparation sodium aluminate solution and goes;
Be dried to powder at 100-300 ℃ at last, get the 4A zeolite product.
Described silicon source is: water glass, water glass, silicon oxide particle, the silicon oxide water-sol or silica gel.
Described aluminium source is: aluminate, alumina gel, metallic aluminium salt.
Described alkali is: sodium hydroxide.
Aforesaid crystallization device is by material inlet, material outlet, the heating medium import, the heating medium outlet is formed, and is materail tube in the middle of it is characterized in that, is heating jacket outside the materail tube, materail tube one end is a material inlet, materail tube the other end material outlet, heating jacket one end is the heating medium import, the heating jacket the other end is the heating medium outlet.
The present invention compared with prior art has following advantage:
Method is simple for technology synthetic zeolite of the present invention, installs for a short time, and cost is low, repeats, and synthetic 4A zeolite has narrower size-grade distribution, quite perfectly crystalline form and high degree of crystallinity, can be continuously produced.
Embodiment:
Fig. 1 is the structural representation of crystallization device of the present invention.
As shown in the figure, the centre is a materail tube 1, is heating jacket 2 outside the materail tube 1, and materail tube 1 one ends are material inlets 3, materail tube 1 the other end material outlet 4, and heating jacket 2 one ends are heating medium imports 5, heating jacket 2 the other ends are heating medium outlets 6.
Embodiment 1
With the water glass sodium silicate solution (Na that is configured to soluble in water
2O:45g/l; SiO
2: 120g/l), sodium aluminate solution is configured to sodium aluminate solution (Na in NaOH solution
2O:90g/l; Al
2O
3: 60g/l).Heating medium enters heating tube 2 from heating medium import 5, flows out from heating medium outlet 6, is warming up to 75 ℃.Above-mentioned two kinds of solution are 2 by silica alumina ratio, enter mixing reactor continuously by pipeline respectively and carry out the hybrid reaction gel, then enter the materail tube 1 of continuous telescoping crystallization device with flow velocity 0.5m/min from material inlet 3, stop 30min at materail tube 1.Flow out from material outlet 4 after the crystallization, remove mother liquor and utilize deionized water wash pH value to 8 by the continuous filtration washing device, the mother liquor under filtering is back to use in the preparation sodium aluminate solution and goes.Be dried to powder through drying plant at 200 ℃ at last and get the 4A zeolite product.
Embodiment 2
With the water glass sodium silicate solution (Na that is configured to soluble in water
2O:75g/l; SiO
2: 180g/l), alumina gel is dissolved in and is configured to sodium aluminate solution (Na in the NaOH solution
2O:70g/l; Al
2O
3: 40g/l).Heating medium enters heating tube 2 from heating medium import 5, flows out from heating medium outlet 6, is warming up to 85 ℃.Above-mentioned two kinds of solution are 5 by silica alumina ratio, enter mixing reactor continuously by pipeline respectively and carry out the hybrid reaction gel, then enter the materail tube 1 of continuous telescoping crystallization device with flow velocity 1m/min from material inlet 3, stop 30min at materail tube 1.Flow out from material outlet 4 after the crystallization, remove mother liquor and utilize deionized water wash pH value to 10 by the continuous filtration washing device, the mother liquor under filtering is back to use in the preparation sodium aluminate solution and goes.Be dried to powder through drying plant at 200 ℃ at last and get the 4A zeolite product.
Silicon oxide particle is dissolved in is configured to sodium silicate solution (Na in the NaOH solution
2O:90g/l; SiO
2: 250g/l), sodium aluminate solution is configured to sodium aluminate solution (Na in NaOH solution
2O:120g/l; Al
2O
3: 40g/l).Heating medium enters heating tube 2 from heating medium import 5, flows out from heating medium outlet 6, is warming up to 95 ℃.Above-mentioned two kinds of solution are 6 by silica alumina ratio, enter mixing reactor continuously by pipeline respectively and carry out the hybrid reaction gel, then enter the materail tube 1 of continuous telescoping crystallization device with flow velocity 0.1m/min from material inlet 3, stop 15min at materail tube 1.Flow out from material outlet 4 after the crystallization, remove mother liquor and utilize deionized water wash pH value to 8 by the continuous filtration washing device, the mother liquor under filtering is back to use in the preparation sodium aluminate solution and goes.Be dried to powder through drying plant at 300 ℃ at last and get the 4A zeolite product.
The silicon oxide water-sol is dissolved in is configured to sodium silicate solution (Na in the NaOH solution
2O:105g/l; SiO
2: 350g/l), alumina gel is dissolved in and is configured to sodium aluminate solution (Na in the NaOH solution
2O:140g/l; Al
2O
3: 60g/l).Heating medium enters heating tube 2 from heating medium import 5, flows out from heating medium outlet 6, is warming up to 60 ℃.Above-mentioned two kinds of solution are 1 by silica alumina ratio, enter mixing reactor continuously by pipeline respectively and carry out the hybrid reaction gel, then enter the materail tube 1 of continuous telescoping crystallization device with flow velocity 10m/min from material inlet 3, stop 60min at materail tube 1.Flow out from material outlet 4 after the crystallization, remove mother liquor and utilize deionized water wash pH value to 8 by the continuous filtration washing device, the mother liquor under filtering is back to use in the preparation sodium aluminate solution and goes.Be dried to powder through drying plant at 200 ℃ at last and get the 4A zeolite product.
Silica gel is dissolved in is configured to sodium silicate solution (Na in the NaOH solution
2O:65g/l; SiO
2: 150g/l), sodium aluminate solution is configured to sodium aluminate solution (Na in NaOH solution
2O:110g/l; Al
2O
3: 60g/l).Heating medium enters heating tube 2 from heating medium import 5, flows out from heating medium outlet 6, is warming up to 100 ℃.Above-mentioned two kinds of solution are 1 by silica alumina ratio, enter mixing reactor continuously by pipeline respectively and carry out the hybrid reaction gel, then enter the materail tube 1 of continuous telescoping crystallization device with flow velocity 0.5m/min from material inlet 3, stop 60min at materail tube 1.Flow out from material outlet 4 after the crystallization, remove mother liquor and utilize deionized water wash pH value to 8 by the continuous filtration washing device, the mother liquor under filtering is back to use in the preparation sodium aluminate solution and goes.Be dried to powder through drying plant at 200 ℃ at last and get the 4A zeolite product.
Claims (4)
1. a technology for preparing the 4A zeolite is characterized in that comprising the steps:
(1) the silicon source is configured to Na in the water-soluble or alkali lye
2O content is 45-105g/l, SiO
2Content is the sodium silicate solution of 120-350g/l; The aluminium source is dissolved in and is configured to Na in the alkali lye
2O content is 70-120g/l, Al
2O
3Content is the sodium aluminate solution of 40-70g/l;
(2) above-mentioned two kinds of solution are 1-6 by silica alumina ratio, enter mixing reactor continuously by pipeline respectively and carry out the hybrid reaction gel, then entering the crystallization device is 60-100 ℃ in temperature, and flow velocity is 0.1-10m/min, and the residence time is to carry out crystallization under the condition of 10-60min;
(3) after the crystallization by continuous filtration, remove mother liquor, and utilize the deionized water wash pH value to 7-11, filter mother liquor down and be back to use to prepare in the sodium aluminate solution and go;
(4) be dried to powder at 100-300 ℃ at last, get the 4A zeolite product.
2. a kind of technology for preparing the 4A zeolite as claimed in claim 1 is characterized in that described silicon source is water glass, water glass, silicon oxide particle, the silicon oxide water-sol or silica gel.
3. a kind of technology for preparing the 4A zeolite as claimed in claim 1 is characterized in that described aluminium source is aluminate, alumina gel or metallic aluminium salt.
4. a kind of technology for preparing the 4A zeolite as claimed in claim 1 is characterized in that described alkali is sodium hydroxide.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03122335 CN1213945C (en) | 2003-04-30 | 2003-04-30 | Technological process and special apparatus for preparing 4A zeolite |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03122335 CN1213945C (en) | 2003-04-30 | 2003-04-30 | Technological process and special apparatus for preparing 4A zeolite |
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| CN1453213A CN1453213A (en) | 2003-11-05 |
| CN1213945C true CN1213945C (en) | 2005-08-10 |
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| CN 03122335 Expired - Fee Related CN1213945C (en) | 2003-04-30 | 2003-04-30 | Technological process and special apparatus for preparing 4A zeolite |
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|---|---|---|---|---|
| CN100577565C (en) * | 2007-08-03 | 2010-01-06 | 中国铝业股份有限公司 | Method for producing 4A zeolite |
| JP6611406B1 (en) * | 2019-05-09 | 2019-11-27 | 株式会社三井Ｅ＆Ｓマシナリー | Method for producing zeolite membrane |
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