CN1105647A - Y zeolite synthetic method - Google Patents
Y zeolite synthetic method Download PDFInfo
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- CN1105647A CN1105647A CN 94100664 CN94100664A CN1105647A CN 1105647 A CN1105647 A CN 1105647A CN 94100664 CN94100664 CN 94100664 CN 94100664 A CN94100664 A CN 94100664A CN 1105647 A CN1105647 A CN 1105647A
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Abstract
The present invention relates to a method for synthesizing Y zeolite. It is characterized by that it is neither different from hydrothermal synthesizing method using chemical product as raw material, nor different from alkali treatment method using natural mineral material as raw material, and it uses an activated argil obtained by using bentonite as raw material and making it pass through the process of sulfuric acid treatment, and then makes the actiated argil pass through the processes of alkali treatment, roasting and crystalizing so as to obtain the invented Y zeolite. Because said method doesn't directly use natural soil minerals and its activated argil particles are very fine, so that the invented product has a small amount of mixed impurity content, and its activity and purity are high, and its cost is low.
Description
The present invention relates to a kind of synthetic method of Y zeolite, present method both had been different from the hydrothermal synthesis method that adopts pure chemistry reagent, was different from the alkaline purification method that adopts original natural earth ore again, but utilized the Y zeolite synthetic method of a kind of treated natural materials for raw material.
Y zeolite (molecular sieve) is commonly used for catalyzer and support of the catalyst.The synthetic of zeolite is broadly divided into two big classes by the raw material difference: be the alkaline purification method of main raw material with the hydrothermal synthesis method of industrial chemicals and with the natural earth ore promptly.
Hydrothermal synthesis method is raw materials used mainly to be silicon-containing compound, aluminum contained compound, alkali and water.The compound of silicon is water glass, silicic acid, silicon sol, halogenated silanes and various active amorphous silica.Prepare zeolite molecular sieve with hydrothermal synthesis method and need consume a large amount of alkali, water glass (water glass) and aluminium hydroxide, make that the molecular sieve cost is higher, for example: the cracking catalyst NaY molecular sieve synthetic method-one ton of molecular sieve reagent of silicate method preparation that extensively adopts with the present Soviet Union consumes 1.48 tons of water glass, 1.35 tons in aluminium hydroxide, 0.5 ton in sodium hydroxide, 0.2 ton in sulfuric acid.
The used raw material of alkaline purification method has natural mineral such as kaolin, wilkinite, diatomite, perlite, volcanic glass.Utilize the alkaline purification method can directly utilize cheap natural resources, adding additives and obtain very high intensity not during moulding, thereby cost is lower, the resulting goods of alkaline purification method contain the solids component of a great deal of, it is more to contain dephasign, its activity and purity all are not so good as to make product with hydrothermal synthesis method, but still are goodish application prospect in promulgated by the State Council economy.China is utilizing kaolin, pyrophyllite, natural nonmetallic minerals synthetic zeolite such as perlite method all has research, do not produce but all form, that is to synthesize Y zeolite because the employing natural mineral is a main raw material, because different places of production material chemical component and physical aspect differ greatly, so can not adopt same processing condition, such as the Ezhou, Hubei has very abundant bentonite resource, its main component is a montmorillonite, be a kind of potential zeolite synthesis places of origin of raw materials, but, be that raw material is difficult to transform the Y zeolite of preparing single phase with the montmorillonite according to foreign literature.The author also carried out test of many times, and the result shows, directly adopts the alkaline purification method to prepare Y zeolite, products therefrom Y zeolite thing phase content very low (less than 50%) with wilkinite.
The objective of the invention is to find out a kind of new Y zeolite synthetic method, if press the different classification of raw material, it neither belongs to the hydrothermal synthesis method that adopts pure chemistry reagent, does not also belong to the alkaline purification method that adopts natural earth ore, and its used main raw material is to be the atlapulgite of main raw material with the wilkinite.Be a kind of synthetic method between above-mentioned two classes, the native ore deposit primary products after promptly suitably handling with process are the synthetic method of raw material.
The synthetic method craft design of Y zeolite of the present invention is as follows:
The first step is carried out the processing of raw material: the natural montmorillonite after will pulverizing is through H
2SO
4Handle, make it to generate high-efficient activated clay, technical indicator is as follows:
SiO
2Content 60-80wt.%
Al
2O
3Content 12-24wt.%
Fe
2O
3Content≤2wt.%
Particle fineness 〉=95%
(200
#Sieve)
Second step was carried out roasting: claim a certain amount of atlapulgite and solid caustic soda NaOH to put into ceramic crucible and mix, add a certain amount of water then and material is mixed well be the gruel shape, send into roasting in the retort furnace.Alkaline earth is than being 1.15-1.3, and water accounts for 18% of gross weight, and maturing temperature is 300-330 ℃.Time is 1-2 hour, the imitation frosted glass furnace cooling.
The 3rd step dissolving: imitation frosted glass taken out in the crucible smash carefully, the back of weighing adds water 250-300ml by per 100 gram imitation frosted glass and soaks dissolving, and soak time is 3 hours, carries out vigorous stirring in the dissolution process, can obtain silicon-aluminum sol.
The 4th step crystallization: resulting silicon-aluminum sol is added about water 1 times (volume ratio), towards rare and stir, promptly can be made into crystallization liquid, the basicity of crystallization liquid is controlled at 2.5-3.2M, by adding water or an amount of crystallization mother liquor is allocated.Crystallization liquid is sent into crystallization in the water bath with thermostatic control after need passing through wearing out of 20-40 hour (20 ℃ of room temperatures).Crystallization temperature is 70-85 ℃, and crystallization time is 24-48 hour, and container can be with hard glass or stainless steel.
The 5th step filtering drying: with crystallization product centrifuging, the oven dry of gained filter cake promptly becomes the Y zeolite powder, and filtrate can be used as crystallization mother liquor and reuses in batching or comprehensively recycle.
Do x-ray diffraction experiment mutually with its thing of finished product that this method makes, compose at 20=6.14 ° 15.61 ° for the X-ray powder diffraction of CuKa line NaY zeolite, 23.58 °, 26.97 °, all there is very strong diffraction peak at places such as 31.31 °, correspond respectively to (111), (331), (533), (624), the diffraction of crystal faces such as (555) proves that the main thing of its finished product is the NaY zeolite mutually, wherein contain a small amount of dephasign, its main component is a NaP type zeolite (GIS).Calculate SiO according to the lattice parameter that X-ray diffraction is measured
2/ Al
2O
3Than being 3.5-4.5.
Present method is not owing to directly use natural earth ore, so what comprise in the product mixes solids component seldom, this has just overcome the impure shortcoming of product greatly, again because the atlapulgite particle is very thin, reactive behavior is bigger, be easy to transform crystal formation through suitable alkaline purification, can obtain to be bordering on the Y zeolite of single phase, improved the activity and the purity of product.Simultaneously, because the atlapulgite cost is lower, price is significantly less than water glass, and chemical reagent such as aluminium hydroxide make present method might have favorable economic benefit.
Embodiment:
Successfully having prepared qualified NaY zeolite with aforesaid method, is the processing condition and the product assay of specific embodiment below.
The embodiment information slip
| Embodiment 1 | Embodiment 2 | Embodiment 3 | |
| The alkaline earth ratio | 1.2 | 1.2 | 1.2 |
| Maturing temperature (℃) | 320 | 330 | 330 |
| Roasting time (hour) | 1.5 | 1.5 | 1.0 |
| Crystallization liquid basicity (M) | 3.0 | 2.7 | 2.0 |
| Digestion time (hour) | 24 | 24 | 46 |
| Crystallization temperature (℃) | 80 | 80 | 80 |
| Crystallization time (hour) | 46 | 40 | 47 |
| Product hygroscopicity value (mg/g) | 258 | 282 | 265 |
| Product Y zeolite lattice parameter (A) | 24.769 | 24.824 | 24.787 |
| SiO 2/Al 2O 3Ratio | 4.3 | 3.8 | 4.1 |
Claims (1)
1, a kind of synthetic method of Y zeolite is characterized in that:
(1) natural montmorillonite after will pulverizing is through H
2SO
4Processing makes it to generate high-efficient activated clay, and technical indicator is:
SiO
2Content 60-80wt.%
Al
2O
3Content 12-24wt.%
Fe
2O
3Content≤2wt.%
Particle fineness 〉=95%
(200
#Sieve)
(2) atlapulgite and solid caustic soda are pressed alkaline earth and account for 18% than being the mixed of 1.15-1.3, water, carry out roasting under 300-330 ℃ of temperature, the time is 1-2 hour,
(3) imitation frosted glass with furnace cooling soaks dissolving in the ratio that 100 grams add 250-300ml water, and the time is 3 hours,
(4) will soak the silicon-aluminum sol that obtains of dissolving and add 1 times in water (volume ratio), basicity is controlled at 2.5-3.2M, allocates by adding an amount of water or crystallization mother liquor, send into crystallization in the water bath with thermostatic control after process 20-40 hour (20 ℃ of room temperatures) is aging, temperature is 70-85 ℃, and the time is 24-48 hour
(5) with crystallization product centrifuging, oven dry.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94100664 CN1105647A (en) | 1994-01-22 | 1994-01-22 | Y zeolite synthetic method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94100664 CN1105647A (en) | 1994-01-22 | 1994-01-22 | Y zeolite synthetic method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1105647A true CN1105647A (en) | 1995-07-26 |
Family
ID=5029771
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 94100664 Pending CN1105647A (en) | 1994-01-22 | 1994-01-22 | Y zeolite synthetic method |
Country Status (1)
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|---|---|
| CN (1) | CN1105647A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101468801B (en) * | 2007-12-27 | 2011-05-18 | 中国石油化工股份有限公司 | Method for preparing Y type molecular sieve containing mesoporous |
| CN102107883B (en) * | 2009-12-23 | 2012-12-26 | 深圳市海川实业股份有限公司 | Method for preparing NaY zeolite |
| CN103230809A (en) * | 2013-04-16 | 2013-08-07 | 中国海洋石油总公司 | Kaolinic heavy aromatic hydrocarbon transalkylation catalyst preparation method |
-
1994
- 1994-01-22 CN CN 94100664 patent/CN1105647A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101468801B (en) * | 2007-12-27 | 2011-05-18 | 中国石油化工股份有限公司 | Method for preparing Y type molecular sieve containing mesoporous |
| CN102107883B (en) * | 2009-12-23 | 2012-12-26 | 深圳市海川实业股份有限公司 | Method for preparing NaY zeolite |
| CN103230809A (en) * | 2013-04-16 | 2013-08-07 | 中国海洋石油总公司 | Kaolinic heavy aromatic hydrocarbon transalkylation catalyst preparation method |
| CN103230809B (en) * | 2013-04-16 | 2015-03-18 | 中国海洋石油总公司 | Kaolinic heavy aromatic hydrocarbon transalkylation catalyst preparation method |
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