CN1448339A - Ammonium ion exchange method of molecular sieve - Google Patents
Ammonium ion exchange method of molecular sieve Download PDFInfo
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- CN1448339A CN1448339A CN 02116277 CN02116277A CN1448339A CN 1448339 A CN1448339 A CN 1448339A CN 02116277 CN02116277 CN 02116277 CN 02116277 A CN02116277 A CN 02116277A CN 1448339 A CN1448339 A CN 1448339A
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Abstract
The ammonium ion exchange process of molecular sieve includes beating the mixture of the molecular sieve and water to obtain slurry; loading the slurry to filtering belt of horizontal belt-type vacuum filtering machine, passing the slurry through one filter cake forming area and one ion exchange area with vacuum liquid acceptors below the belt, washing, sucking to dry filter cake and unloading the filter cake. The molecular sieve is Y-type molecular sieve, the slurry contains also alkali or alkali-salt mixture with alkali content of 0.1-8 wt% and salt content of 0-5 wt%, the liquid acceptor in the filter cake forming area has such vacuum degree that no chap is formed in the filter cake, and ammonium ion solution is added from the upper part of filter cake in the ion exchange area with the solution concentration and use amount and the liquid acceptor vacuum degree in the ion exchange area being such that the ultimate Y-type molecular sieve has sodium oxide content not higher than 1.5 w.
Description
Invention field
The invention relates to a kind of ion-exchange techniques of molecular sieve, more specifically say so about a kind of ammonium ion exchange method of molecular sieve.
Background technology
Y zeolite is the active ingredient commonly used of catalyzer, in the catalyzer, prepares by the NaY molecular sieve as Y zeolite contained in the hydrocarbon cracking catalyzer.NaY molecular sieve and the aqueous solution that contains ammonium ion and/or rare earth ion are carried out ion-exchange, washing, Y zeolite dry and that roasting obtains to be commonly referred to one and to hand over a roasting Y zeolite.It comprises that one hands over a roasting super-stable Y molecular sieves USY, to hand over a roasting rare earth Y type molecular sieve REY, to hand over a roasting rare earth hydrogen Y zeolite REHY and to hand over a roasting hydrogen Y molecular sieve HY.The lattice constant of one friendship, one roasting Y zeolite is the 24.48-24.66 dust, and sodium oxide content is the heavy % of 3-5.One hands over the sodium content in the roasting Y zeolite still higher, can not still need to carry out ion-exchange to reduce sodium content wherein and/or to introduce rare earth ion or other ion directly as the active ingredient of cracking catalyst.
At present, industrially Y zeolite is carried out ammonium ion exchange two kinds of methods are arranged.
First method is with Y zeolite and the aqueous solution making beating that contains ammonium ion, carries out ion-exchange, filtration, washing, drying, roasting or not roasting, and the sheet frame filter is adopted in filtration wherein.The shortcoming that adopts this method is that efficient is low, and the water consumption is big.
Second method is that Y zeolite is mixed the aqueous slurry that making beating forms a kind of Y zeolite with water, these slurries directly are loaded on the transition band of band filter, on transition band, form one deck filter cake, then, add the aqueous solution that contains ammonium ion from filter cake top, under the vacuum action of bottom vacuum chamber, the solution that contains ammonium ion passes through filter cake continuously.The advantage of using band filter is can integrate solid-liquid separation, washing, exchange, filter, the efficient height, and the water consumption is little.
US 3,943,233 disclose the method for a large amount of trickle solid particles of a kind of continuous processing, this method comprises that the slurries with a kind of fine solid particle are supplied to a continuous mobile and horizontal band filter, this band filter is equipped with a vacuum chamber with part separated from each other, wherein, each part separated from each other with one independently the liquid susceptor link to each other with vacuum controller.On the transition band slurries, impose enough vacuum, obtain containing in a kind of particulate space the filter cake thin layer of the lubricous dry of water, when filter cake passes through described vacuum chamber continuously, it can be contacted with the solution of described particle generation mass trnsfer reaction with a kind of, simultaneously, vacuum degree control can be formed an immobilized liquid Xiao Chi on filter cake, after from filter cake, flowing down enough liquid, form a kind of smoothly, the surface does not have be full of cracks, contains the filter cake of liquid between the filter cake particle, on filter cake, add another kind of liquid, and control enough vacuum tightness, and make liquid flow through filter cake fast, unload filter cake from strainer.
US 3,943, but 233 also disclose a kind of method of carrying out ion-exchange continuously of fluidization zeolite granular, this method comprises described zeolite granular and first kind of liquid making beating, these slurries are loaded into the infeed end of a continuous horizontal belt vacuum filter with the speed of substantially constant, move the transition band that slurry is housed continuously, order forms the district by a filter cake, at least one ion-exchange area and a washing section, simultaneously independently impose vacuum on the liquid receiver under the transition band, unload filter cake from transition band at each.The method is characterized in that filter cake does not have check surface basically when leaving filter cake formation district, but can contain liquid between the space of fluidised zeolite granular, in the ion exchange treatment process, filter cake is at ion-exchange area, under filtration condition, contact with a kind of ion-exchange liquids, mode with a kind of filter cake is left ion-exchange area, this filter cake is smooth, basically there is not check surface, can contain liquid between the space of fluidised zeolite granular, and under vacuum, wash the filter cake after the ion-exchange fast.
Experiment shows that US 3,943,233 described methods are applicable to ion-exchange, the washing process of some big solid particulates and part zeolite.But, because one hands in the aqueous slurry of a roasting Y zeolite, the very tiny and reason of handing over roasting Y zeolite self inherent nature of the particle of molecular sieve, after slurries of handing over a roasting Y zeolite to mix making beating formation with water are loaded the transition band of going up band filter, formed filter cake is a kind of very filter cake of densification, perviousness extreme difference, and filtration velocity (liquid sees through the speed of filter cake) is very slow.When carrying out ammonium ion exchange, the solution that contains ammonium ion adds from filter cake top, and the speed that sees through filter cake is slower, and the ammonium ion exchange process can't be carried out.Therefore, still on band filter, do not hand over a roasting y-type zeolite to carry out the method for ammonium ion exchange in the prior art to one.
Summary of the invention
The purpose of this invention is to provide a kind of new not only water-saving efficient but also high molecular sieve ammonium ion exchange method.
Molecular sieve ammonium ion exchange method provided by the invention comprises pulls an oar a kind of molecular sieve with water, the slurries that obtain are loaded on the strainer of horizontal vacuum belt filter continuously, order forms district and an ion-exchange area by a filter cake, impose vacuum in the liquid receiver under filter cake formation district and ion-exchange area transition band, washing, blot filter cake, unload filter cake from transition band, wherein, described molecular sieve is a friendship one a roasting Y zeolite, the mixture that has also added alkali or alkali and salt in the described slurries, the consumption of described alkali is the heavy % of the 0.1-8 of molecular sieve consumption, the consumption of salt is the heavy % of the 0-5 of molecular sieve consumption, and the vacuum tightness that described filter cake forms in district's liquid receiver guarantees that filter cake does not have be full of cracks substantially; At described ion-exchange area, add the solution that contains ammonium ion on the top of filter cake, sodium oxide content is not higher than 1.5 heavy % in the Y zeolite that the vacuum tightness that contains concentration, consumption and the ion-exchange area liquid receiver of the solution of ammonium ion guarantees finally to obtain.
Compared with prior art, method provided by the invention has overcome prior art and can not hand over a roasting Y zeolite to carry out the shortcoming of ammonium ion exchange to one on band filter, has successfully realized handing over a roasting Y zeolite to carry out ammonium ion exchange to one on band filter.Method provided by the invention has the advantage of using band filter certainly, and promptly the water consumption is little, the advantage that efficient is high.
Fig. 1 is the schematic flow sheet of the method for the invention.
Embodiment
According to method provided by the invention, described one hands over a roasting Y zeolite to comprise that one hands over a roasting ultra-steady Y molecular sieve USY, one hands over a roasting rare-earth Y molecular sieve REY, to hand over a roasting rare earth hydrogen Y molecular sieve REHY and to hand over a roasting hydrogen Y molecular sieve HY, and these molecular sieves and preparation method thereof are conventionally known to one of skill in the art.Handing over a roasting hydrogen Y molecular sieve with one is example, and its preparation method is normally with the sodium Y molecular sieve and the aqueous solution that contains ammonium ion, as ammonium chloride, ammonium sulfate solution mixing carrying out ion-exchange, washing, dry and roasting.Wherein, contain the concentration of the aqueous solution of ammonium ion and consumption and give-and-take conditions also for conventionally known to one of skill in the art, as in ammonium salt, the concentration that contains the aqueous solution of ammonium ion is generally the 50-300 grams per liter, be preferably the 100-200 grams per liter, the temperature of exchange is a room temperature to 100 ℃, is preferably 50-90 ℃, the time of exchange is 0.5-2 hour, is preferably 0.5-1 hour.Condition dry and roasting is conventionally known to one of skill in the art, is room temperature to 200 ℃ as the exsiccant temperature, is preferably 100-150 ℃, and maturing temperature is 500-800 ℃, is preferably 600-700 ℃, and roasting time is 1-3 hour, is preferably 2-3 hour.One hands over a roasting Y zeolite to have following common character: lattice constant is the 24.48-24.66 dust, and sodium oxide content is the heavy % of 3-5.
Described one hands over a roasting Y zeolite also to be available commercially by existing method preparation.
Described alkali is selected from water soluble, and does not form in sedimentary various mineral alkalis and the organic bases one or more in the ion exchange process that carries out subsequently, washing process, as ammoniacal liquor, alkali-metal oxyhydroxide, one or more in the organic amine.Because ammoniacal liquor, sodium hydroxide cheaply are easy to get, and in system, do not introduce the new ion that can not remove, therefore, preferred ammoniacal liquor and/or sodium hydroxide.The consumption of described alkali is the heavy % of the 0.1-8 of molecular sieve consumption, is preferably the heavy % of 0.5-5.
Described salt refers to water-soluble and does not generate in the sedimentary various salt one or more with alkali, as in ammonium and alkali-metal hydrochloride, vitriol, the nitrate one or more, as in ammonium chloride, ammonium sulfate, ammonium nitrate, sodium sulfate, sodium-chlor, the SODIUMNITRATE one or more.In order to make full use of resource, described salt can and preferably use ammonium exchange waste liquid, and the solution and the molecular sieve that promptly contain ammonium ion carry out the waste liquid that the ion-exchange after-filtration obtains.The consumption of described salt is the heavy % of the 0-5 of molecular sieve consumption, is preferably the heavy % of 0-3.
In the slurries that described molecular sieve and water making beating form, the content range of molecular sieve is conventional content range, and in general, the content of molecular sieve is the 100-300 grams per liter in the slurries.
During filtration, the temperature of described slurries can be 5-100 ℃, is preferably 50-90 ℃.
According to specific embodiment of the present invention, can be by flow implementation the present invention shown in Figure 1.
One, filter cake forms
With 5-100 ℃, the molecular sieve pulp of preferred 50-90 ℃ the mixture that contains alkali or alkali and salt is loaded on the transition band 3 of horizontal vacuum band-type filter machine continuously by pipeline 2 from making beating jar 1, the consumption of described alkali is the heavy % of the 0.1-8 of molecular sieve consumption, be preferably the heavy % of 0.5-5, the consumption of described salt is the heavy % of the 0-5 of molecular sieve consumption, is preferably the heavy % of 0-3.Transition band 3 rotates by filter cake continuously and forms district 4, the liquid receiver 5 that filter cake forms district 4 be positioned at transition band 3 below, liquid receiver 5 is vacuumized, under the effect of vacuum, liquid in the slurries on the transition band 3 enters in the liquid receiver 5 by filter cloth, and the waste liquid in the liquid receiver 5 is by pipeline 6 dischargings.Simultaneously, the slurries on transition band 3 form filter cake gradually, and the concentration of slurries and loading speed should guarantee that the thickness of the filter cake that forms is no more than 20 millimeters, is preferably the 5-15 millimeter.Vacuum tightness in the liquid receiver 5 should make filter cake not have be full of cracks substantially.Vacuum tightness in the liquid receiver 5 is generally the 0.01-0.08 MPa, is preferably the 0.02-0.07 MPa.
Wherein, the exchange waste liquid that described salt can be obtained by the ion-exchange area 7 of the following stated provides, promptly additionally do not add salt, directly hand over a roasting Y zeolite, alkali and water to mix making beating, make the described slurries that contain molecular sieve with the exchange waste liquid in the liquid receiver 8 and.This has reduced the consumption of salt on the one hand and has reduced the water consumption, has also reduced the sewage emissions amount on the other hand.
Two, ammonium ion exchange
The filter cake that forms district's 4 formation at filter cake enters ion-exchange area 7, the liquid receiver 8 of ion-exchange area 7 is positioned at the below of transition band 3, liquid receiver 8 is vacuumized, and above filter cake, add 5-100 ℃ by pipeline 10 by container 9, preferred 50-90 ℃ the aqueous solution that contains ammonium ion, under vacuum action, when the aqueous solution that contains ammonium ion sees through filter cake constantly and molecular sieve generation ammonium ion exchange.
Wherein, the vacuum tightness in the liquid receiver 8 should make the filter cake surface keep the moistening be full of cracks that do not occur.In ammonium salt, the concentration that contains the solution of ammonium ion is the 30-100 grams per liter, is preferably the 50-100 grams per liter, and it is 0.1-0.8 that the consumption of ammonium salt makes the weight ratio of ammonium salt and molecular sieve, is preferably 0.2-0.6.The precursor of described ammonium ion, promptly ammonium salt is selected from one or more in the various solubility ammonium salts, as, one or more in ammonium chloride, ammonium sulfate, ammonium nitrate, the ammonium phosphate.The described temperature that contains ammonium ion solution is 5-100 ℃, is preferably 50-90 ℃.
The exchange waste liquid that obtains in the liquid receiver 8 except be used for molecular sieve making beating, can also mix (fresh here ammonium ion exchange liquid refers to the aqueous solution that contains ammonium ion that ammonium concentration is higher) with fresh ammonium ion exchange liquid, or directly dissolve ammonium salt and make exchange liquid, be the described aqueous solution that contains ammonium ion, the waste liquid in the liquid receiver 8 is by pipeline 11 dischargings.
Three. washing
Mode of washing is conventionally known to one of skill in the art, adds deionized water from container 12 through pipeline 13 on the filter cake that comes from ion-exchange area, simultaneously, liquid receiver 14 is vacuumized, under vacuum action, deionized water sees through filter cake, with the acid ion flush away in the filter cake.The weight ratio of deionized water and molecular sieve is generally 1-15, is preferably 2-10.The temperature of deionized water is 5-100 ℃, is preferably 20-90 ℃.
The waste liquid that liquid receiver 14 is collected is discharged through pipeline 15, with liquid mixing in the liquid receiver 16 or do not mix, is used for preparing fresh exchange liquid, also can be used for mixing with fresh exchange liquid, then as exchanging liquid.Vacuum tightness in the liquid receiver 14 is generally the 0.01-0.08 MPa, is preferably the 0.02-0.07 MPa.
Four. blot
The method that blots is conventionally known to one of skill in the art, and under the effect of vacuum, the liquid in the filter cake is drawn out of in the liquid receiver 16 of the filter cake after the washing under transition band 3.Liquid in the liquid receiver 16 is discharged through pipeline 17, and liquid phase together in purposes and the receptor 14.Vacuum tightness in the liquid receiver 16 is the 0.01-0.08 MPa, is preferably the 0.02-0.07 MPa.
Five. unload the filter cake after blotting at last.
The following examples will the present invention will be further described.
Following example adopts B suction filtration device to experimentize, and method provided by the invention is described.Because when adopting B suction filtration device, the stage such as also experienced filter cake formation, ammonium ion exchange, wash, blot, though these steps separately carry out, different with the mode of carrying out continuously on the band filter.But employing B suction filtration device experimentizes and adopts band filter to experimentize, and no matter still is being all to be of equal value on effect on the process.
Example 1
This example illustrates method provided by the invention.
With 30 grams one hand over a roasting rare earth hydrogen Y molecular sieve (rare earth oxide content is 2.0 heavy %, wherein, La
2O
3Content is 1.7 heavy %, CeO
2Content is 0.2 heavy %, other rare-earth oxide content is 0.1 heavy %, sodium oxide content is 4.6 heavy %, lattice constant is 24.63 dusts, Lanzhou refinery company catalyst plant is produced), deionized water and sodium hydroxide (chemical pure) are pulled an oar together, the content that makes molecular sieve in the slurries that obtain is 200 grams per liters, sodium hydroxide concentration is 1 heavy % of molecular sieve, under agitation be heated to 80 ℃, the slurries that obtain are poured on the filter cloth of a B, filter flask is evacuated to 0.03 MPa, under this vacuum, filter until the absence of liquid existence of filter cake surface, the linear velocity that recording liquid descends is called separating and filtering speed here.
Adding 100 ml concns on filter cake is the ammonium chloride solution of 100 grams per liters, ammonium chloride solution when seeing through filter cake with filter cake in molecular sieve carried out ammonium ion exchange, absence of liquid exists until the filter cake surface.The linear velocity that recording liquid descends is called the exchange filtration velocity here.
Add 80 ml deionized water on filter cake filter cake is washed, absence of liquid exists until the filter cake surface, and the linear velocity that recording liquid descends is called washing and filtering speed here.
Separating and filtering speed, exchange filtration velocity and washing and filtering speed are as shown in table 1.In 120 ℃ of oven dry, with aas determination sodium oxide content wherein, the results are shown in Table 2 with filter cake.
Example 2
This example illustrates method provided by the invention.
Press the method for example 1 and hand over a roasting rare earth hydrogen Y molecular sieve making beating one, filter, exchange, wash and record separating and filtering speed, exchange filtration velocity and washing and filtering speed, different is to replace sodium hydroxide with 25 strong aquas that weigh %, and it is 3 heavy % of molecular sieve consumption that the consumption of strong aqua makes the consumption of ammonia.The result lists in respectively in table 1 and 2.
Example 3
This example illustrates method provided by the invention.
The method of pressing example 1 is handed over a roasting rare earth hydrogen Y molecular sieve making beating with one, filters, exchange, washing also record separating and filtering speed, exchange filtration velocity and washing and filtering speed, and the rare earth oxide content of different is used rare earth hydrogen Y molecular sieve is 7.0 heavy %, wherein La
2O
3Content is 2.3 heavy %, CeO
2Content is 4.1 heavy %, and other rare earth oxide content is 0.6 heavy %, and sodium oxide content is 4.0 heavy %, and the content of molecular sieve is 150 grams per liters in the slurries.The result lists in respectively in table 1 and 2.
Example 4
This example illustrates method provided by the invention.
The method of pressing example 1 is handed over a roasting rare earth hydrogen Y molecular sieve making beating with one, filters, exchange, washing also record separating and filtering speed, exchange filtration velocity and washing and filtering speed, and the rare earth oxide content of different is used rare earth hydrogen Y molecular sieve is 5.0 heavy %, wherein La
2O
3Content is 1.7 heavy %, CeO
2Content is 3.0 heavy %, and other rare earth oxide content is 0.3 heavy %, and sodium oxide content is 4.0 heavy %, and has added the ammonium chloride that accounts for molecular sieve consumption 1 heavy %, the temperature to 70 of heating slurries ℃.The result lists in respectively in table 1 and 2.
Comparative Examples 1
Filter method when this Comparative Examples explanation does not add the mixture of alkali or alkali and salt.
Press the method for example 1 and hand over a roasting rare earth hydrogen Y molecular sieve making beating one, filtration, exchange, washing and record separating and filtering speed, exchange filtration velocity and washing and filtering speed, different does not just add sodium hydroxide, and the result lists in respectively in table 1 and 2.
Table 1
| Example number | Separating and filtering speed, cm per minute | The exchange filtration velocity, cm per minute | Washing and filtering speed, cm per |
| 1 | ????2.63 | ?????0.37 | ?????0.32 |
| 2 | ????1.64 | ?????0.27 | ?????0.24 |
| 3 | ????2.32 | ?????0.28 | ?????0.27 |
| 4 | ????2.30 | ?????0.30 | ?????0.27 |
| Comparative Examples 1 | ????0.86 | ?????0.15 | ?????0.14 |
The result of table 1 shows, adopts method provided by the invention, hands over the mixture that adds alkali or alkali and salt in the roasting molecular sieve pulp can improve the filtration velocity of molecular sieve aqueous slurry greatly one.Adopt method provided by the invention, separating and filtering speed is 1.9-3.1 times of prior art, and the exchange filtration velocity is 1.8-2.5 a times of prior art, and washing and filtering speed is 1.7-2.3 times of prior art.This has solved puzzlement those skilled in the art problem for many years, promptly one hands over a roasting Y zeolite aqueous slurry filtration velocity slow, the problem that can not carry out ion-exchange on band filter.
Table 2
| Example number | Sodium oxide content, heavy % |
| ????1 | ?????1.0 |
| ????2 | ?????0.9 |
| ????3 | ?????0.9 |
| ????4 | ?????0.8 |
| Comparative Examples 1 | ?????1.0 |
The result of table 2 shows that even add sodium hydroxide, owing to have ion-exchange and washing process behind the separating and filtering, sodium oxide content can not raise yet in the product.
Example 5
This example illustrates the applicable cases of method provided by the invention on the technical scale band filter.
By flow process shown in Figure 1, hand over a roasting rare earth hydrogen Y molecular sieve, sodium hydroxide and deionized water in making beating jar 1, to mix making beating example 1 described, obtain containing the molecular sieve pulp of molecular sieve 150 grams per liters, the consumption of sodium hydroxide is 0.5 heavy % of molecular sieve consumption.When the amount of the exchange waste liquid that produces in the liquid receiver 8 is enough, partly replace deionized water with this waste liquid, it is 1.9 heavy % of molecular sieve consumption that the consumption of waste liquid makes institute's saliniferous amount in the slurries, the slurries that obtain are heated to 80 ℃, be loaded into continuously on the vacuum band 3 of a horizontal vacuum band-type filter machine by pipeline 2 then, transition band 3 rotates continuously, make the slurries on the transition band 3 enter the filter cake formation district 4 that is connected with liquid receiver 5, the vacuum tightness of liquid receiver 5 is 0.05 MPa, form district 4 by filter cake, the slurries formation thickness on the transition band 3 is 10 millimeters filter cake.The filter cake surface does not have be full of cracks, and waste liquid is collected in liquid receiver 5, and by pipeline 6 dischargings.
Along with moving of transition band 3, form the filter cake that forms in the district 4 at filter cake and enter the ion-exchange area 7 that liquid receiver 8 is housed, the vacuum tightness in the liquid receiver 8 is 0.05 MPa, from the container 9 on filter cake top by pipeline 10 with 3 meters
3/ hour flow, adding temperature is 60 ℃ of aqueous ammonium chloride solutions that concentration is 50 grams per liters, it is 0.2 that described aqueous ammonium chloride solution consumption makes ammonium chloride and molecular sieve weight ratio, exchange waste liquid in the liquid receiver 8 is discharged by pipeline 11, a part wherein is used for joining making beating jar 1, as the source of described salt.Remainder mixes with fresh ammonium chloride solution, and being made into as mentioned above, concentration is the ammonium chloride exchange fluid of 50 grams per liters.
Along with moving of strainer 3, the exchange fluid exchange is the scrub raffinate that obtains of following liquid receiver 14 and the mixed solution of fresh ammonium chloride solution, the concentration of ammonium chloride is 56 grams per liters in this mixed solution, and it is 0.2 that the consumption of this mixed solution makes wherein ammonium chloride and molecular sieve weight ratio.
Along with moving of strainer 3, leave ion-exchange area 7, container 12 from filter cake top, adding temperature by pipeline 13 is 80 ℃ deionized water, under the vacuum action, liquid sees through filter cake, washes out foreign ion wherein in 3 times liquid receivers 14 of transition band, the deionized water consumption is 4 times of molecular sieve consumption, and the vacuum tightness in the liquid receiver 14 is 0.05 MPa.Scrub raffinate in the liquid receiver 14 from pipeline 15 discharge and with liquid mixing from liquid receiver 16, be used for being mixed with into the exchange liquid that above-mentioned ammonium chloride concentration is 56 grams per liters with fresh ammonium chloride solution.
After washing finished, filter cake continued to move ahead under the drive of transition band 3, and under the vacuum action, the liquid in the filter cake is by further sucking-off in liquid receiver 16, and the vacuum tightness in the liquid receiver 16 is 0.05 MPa.Unload filter cake, 120 ℃ of oven dry obtain Y zeolite, and it changes sodium content is 0.9 heavy %.Liquid in the liquid receiver 16 is discharged with the scrub raffinate that obtains in the liquid receiver 14 from pipeline 17 and is mixed.
Claims (15)
1. the ammonium ion exchange method of a molecular sieve, this method comprises pulls an oar a kind of molecular sieve with water, the slurries that obtain are loaded on the strainer of horizontal vacuum belt filter continuously, order forms district and an ion-exchange area by a filter cake, impose vacuum in the liquid receiver under filter cake formation district and ion-exchange area transition band, washing, blot filter cake, unload filter cake from transition band, it is characterized in that, described molecular sieve is a friendship one a roasting Y zeolite, the mixture that has also added alkali or alkali and salt in the described slurries, the consumption of described alkali is the heavy % of the 0.1-8 of molecular sieve consumption, the consumption of salt is the heavy % of the 0-5 of molecular sieve consumption, and the vacuum tightness that described filter cake forms in district's liquid receiver guarantees that filter cake does not have be full of cracks substantially; At described ion-exchange area, add the solution that contains ammonium ion on the top of filter cake, sodium oxide content is not higher than 1.5 heavy % in the Y zeolite that the vacuum tightness that contains concentration, consumption and the ion-exchange area liquid receiver of the solution of ammonium ion guarantees finally to obtain.
2. method according to claim 1 is characterized in that, described one hands over a roasting Y zeolite to comprise that one hands over a roasting ultra-steady Y molecular sieve, and one hands over a roasting rare-earth Y molecular sieve, to hand over a roasting rare earth hydrogen Y molecular sieve and to hand over a roasting hydrogen Y molecular sieve.
3. method according to claim 1 is characterized in that, described one hands over a roasting Y zeolite to refer to that one hands over a roasting rare-earth Y molecular sieve and/or to hand over a roasting rare earth hydrogen Y molecular sieve.
4. method according to claim 1 is characterized in that, described alkali is selected from ammoniacal liquor, alkali-metal oxyhydroxide, one or more in the organic amine.
5. method according to claim 4 is characterized in that described alkali is selected from ammoniacal liquor and/or sodium hydroxide.
6. method according to claim 1 is characterized in that, the consumption of described alkali is the heavy % of the 0.5-5 of molecular sieve consumption.
7. method according to claim 1 is characterized in that, described salt is selected from one or more in ammonium and alkali-metal hydrochloride, vitriol, the nitrate.
8. method according to claim 7 is characterized in that described salt is selected from one or more in ammonium chloride, ammonium sulfate, ammonium nitrate, sodium sulfate, sodium-chlor, the SODIUMNITRATE.
9. method according to claim 1 is characterized in that, described salt is from the exchange waste liquid of ion-exchange area.
10. method according to claim 1 is characterized in that, the consumption of described salt is the heavy % of the 0-3 of molecular sieve consumption.
11. method according to claim 1 is characterized in that, in the slurries that described molecular sieve and water making beating form, the content of molecular sieve is the 100-300 grams per liter.
12. method according to claim 1 is characterized in that, the temperature of described slurries is 50-90 ℃.
13. method according to claim 1 is characterized in that, the vacuum tightness in the liquid receiver under filter cake formation district and the ion-exchange area transition band is the 0.01-0.08 MPa.
14. method according to claim 1 is characterized in that, the described temperature that contains the solution of ammonium ion is 5-100 ℃, and in ammonium salt, the concentration that contains the solution of ammonium ion is the 30-100 grams per liter.
15. method according to claim 14 is characterized in that, the described temperature that contains the solution of ammonium ion is 50-90 ℃, and the concentration that contains the solution of ammonium ion is the 50-100 grams per liter.
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| CNB021162778A CN1176019C (en) | 2002-03-29 | 2002-03-29 | Ammonium ion exchange method of molecular sieve |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100404134C (en) * | 2005-08-09 | 2008-07-23 | 中国石油化工股份有限公司 | Ammonium ion exchange method of NaY molecular sieve |
| CN102749350A (en) * | 2011-04-20 | 2012-10-24 | 中国石油化工股份有限公司 | Method for determining desorption heat effect of organic adsorbate on molecular sieve |
| CN102749261A (en) * | 2011-04-20 | 2012-10-24 | 中国石油化工股份有限公司 | Method for determining molecular sieve and adsorbate affinity AT value |
| CN101518749B (en) * | 2009-03-05 | 2013-06-26 | 华东理工大学 | Ion exchange process for multistage reverse flow zeolite molecular sieve of band filter |
| CN103691491A (en) * | 2013-12-31 | 2014-04-02 | 中国天辰工程有限公司 | Method for removing sodium by silicon-aluminum-phosphor molecular sieve catalyst |
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2002
- 2002-03-29 CN CNB021162778A patent/CN1176019C/en not_active Expired - Lifetime
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100404134C (en) * | 2005-08-09 | 2008-07-23 | 中国石油化工股份有限公司 | Ammonium ion exchange method of NaY molecular sieve |
| CN101518749B (en) * | 2009-03-05 | 2013-06-26 | 华东理工大学 | Ion exchange process for multistage reverse flow zeolite molecular sieve of band filter |
| CN102749350A (en) * | 2011-04-20 | 2012-10-24 | 中国石油化工股份有限公司 | Method for determining desorption heat effect of organic adsorbate on molecular sieve |
| CN102749261A (en) * | 2011-04-20 | 2012-10-24 | 中国石油化工股份有限公司 | Method for determining molecular sieve and adsorbate affinity AT value |
| CN103691491A (en) * | 2013-12-31 | 2014-04-02 | 中国天辰工程有限公司 | Method for removing sodium by silicon-aluminum-phosphor molecular sieve catalyst |
| CN103691491B (en) * | 2013-12-31 | 2015-07-22 | 中国天辰工程有限公司 | Method for removing sodium by silicon-aluminum-phosphor molecular sieve catalyst |
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