CN1195676C - Molecular sieve ammonium ion exchange process - Google Patents
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- CN1195676C CN1195676C CNB011342757A CN01134275A CN1195676C CN 1195676 C CN1195676 C CN 1195676C CN B011342757 A CNB011342757 A CN B011342757A CN 01134275 A CN01134275 A CN 01134275A CN 1195676 C CN1195676 C CN 1195676C
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Abstract
The present invention relates to an ammonium ion exchange method of a molecular sieve, which comprises the following steps: a molecular sieve and water are pulped together; an obtained serous fluid is continuously loaded on the filter belt of a horizontal belt vacuum filter and sequentially passes through a filter cake forming region and an ion exchange region; a liquid receiver under the filter belt of the filter cake forming region and the ion exchange region is vacuumized, a filter cake is washed, sucked dry and detached from the filter belt, wherein the molecular sieve is a Y-shaped molecular sieve of one-step exchange and one-step roasting. Acid and/or salt are/is also added to the serous fluid, and the dosage of the acid and/or the salt is 0.1 to 5 wt% of that of the molecular sieve. The vacuum degree of the liquid receiver in the filter cake forming region can ensure that no crack basically exists on the surface of the filter cake. In the ion exchange region, a solution containing ammonium ions is added to the upper part of the filter cake, the concentration and the dosage of the solution containing the ammonium ions and the vacuum degree of the liquid receiver in the ion exchange region ensure that the sodium oxide content of the finally obtained Y-shaped molecular sieve is not higher than 1.5 wt%.
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.Sodium Y 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 3-5 weight %.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 ions 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, the solution that contains ammonium ion passes through filter cake continuously in the vacuum chamber of bottom.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 mobile continuous 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, and 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, also added acid and/or salt in the described slurries, the consumption of described acid and/or salt is the 0.1-5 weight % of molecular sieve consumption.The vacuum tightness that described filter cake forms in district's liquid receiver guarantees that filter cake does not have be full of cracks on the surface substantially when leaving filter cake formation district; 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 weight % 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.
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 of the ammonium ion aqueous solution 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 3-5 weight %.
Described one hands over a roasting Y zeolite also to be available commercially by existing method preparation.
Described acid is selected from one or more in water-soluble acid, comprise in water-soluble mineral acid and the organic acid one or more, example hydrochloric acid, nitric acid, phosphoric acid, formic acid, acetate, propionic acid, phenylformic acid etc. wherein, are preferably hydrochloric acid, sulfuric acid, nitric acid and/or phosphoric acid.
Described salt refers to one or more in water-soluble various salt, as in the soluble salt hydrochlorate of ammonium, basic metal, aluminium, iron, rare earth, vitriol, nitrate, the phosphoric acid salt one or more, wherein, be preferably in hydrochloride, vitriol and the nitrate of basic metal, ammonium, iron, rare earth metal one or more, as in the muriate of ammonium chloride, ammonium sulfate, ammonium nitrate, ammonium phosphate, sodium sulfate, sodium-chlor, SODIUMNITRATE and rare earth metal one or more.
The consumption of described acid and/or salt is the 0.1-5 weight % of molecular sieve consumption, is preferably 0.5-3 weight %.
In the slurries that described molecular sieve and water making beating obtain, the content range of molecular sieve is conventionally known to one of skill in the art, and the content of molecular sieve is generally the 100-300 grams per liter in the described slurries.The temperature of described slurries can be 5-100 ℃, is preferably 50-90 ℃.
According to embodiment preferred of the present invention, can be by flow implementation the present invention shown in Figure 1.
One, filter cake forms
With 5-100 ℃, preferred 50-90 ℃ the molecular sieve pulp that contains acid and/or salt is loaded on the transition band 3 of horizontal vacuum band-type filter machine continuously by pipeline 2 from making beating jar 1, 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, the 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 does not have be full of cracks substantially on the filter cake surface.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 acid and/or salt can be obtained by the ion-exchange area 7 of the following stated provides, promptly additionally do not add acid and/or salt, directly hand over a roasting Y zeolite and water to mix making beating, make the described slurries that contain molecular sieve with the exchange waste liquid in the liquid receiver 8 in the ion-exchange area 7 and.This has reduced the consumption of acid and/or salt on the one hand and has reduced the water consumption, has also reduced the sewage emissions amount.
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 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 ion-exchange area obtains, simultaneously, liquid receiver 14 is vacuumized, under vacuum action, liquid 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, can be used to prepare fresh exchange liquid, also can be used for mixing with fresh exchange liquid, then as exchange 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.
Comparative Examples 1
The existing ammonium ion exchange method of this Comparative Examples explanation.
(lattice constant is 24.52 dusts to hand over a roasting ultra-steady Y molecular sieve with one, sodium oxide content is 4.3 weight %, Qilu Petrochemical company catalyst plant is produced), ammonium chloride and deionized water are pressed molecular sieve (butt): ammonium chloride: the weight ratio of water=1: 0.3: 15 is mixed making beating, be warming up to 90 ℃, under agitation carried out ion-exchange 60 minutes, filter, be not detected to there being chlorion with the deionized water wash filter cake, the waste liquid A1 that obtains is standby.Filter cake obtains ultra-steady Y molecular sieve B1 through 120 ℃ of oven dry, and sodium oxide content is 0.9 weight % among the B1.In ammonium chloride, the ammonium concentration among the waste liquid A1 is about 20 grams per liters, and in sodium-chlor, Na ion concentration is about 7 grams per liters.
Wherein, sodium oxide content adopts aas determination in the molecular sieve, and ammonium concentration and Na ion concentration are got by calculating among the waste liquid A1.
Comparative Examples 2
The existing ammonium ion exchange method of this Comparative Examples explanation.
Method by Comparative Examples 1 is carried out ammonium ion exchange, washing, drying, different used molecular sieves is that (lattice constant is 24.6 dusts to a friendship one roasting hydrogen Y molecular sieve, sodium oxide content is 4.5 weight %, and Qilu Petrochemical company catalyst plant is produced), obtain the standby and Y zeolite B2 of waste liquid A2.In ammonium chloride, the ammonium concentration among the waste liquid A2 is about 25 grams per liters, is about 7 grams per liters in the sodium-chlor Na ion concentration.Sodium oxide content among the Y zeolite B2 is 1.0 weight %
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, just these steps are separately carried out, and be of equal value to the mode of carrying out continuously on the band filter.Therefore, 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
Comparative Examples 1 described one is handed over roasting ultra-steady Y molecular sieve, deionized water and Comparative Examples 1 a described waste liquid A1, mix making beating, making molecular sieve content is the slurries that contain molecular sieve of 120 grams per liters, wherein, the consumption of salt (being contained ammonium chloride and sodium-chlor among the used waste liquid A1) is 1.1 weight % of molecular sieve consumption.The molecular sieve pulp that obtains is heated to 90 ℃, pours in the B, simultaneously, filter flask is evacuated to 0.07 MPa.On filter cloth, form thickness and be about 10 millimeters filter cake.When the absence of liquid of filter cake surface, adding concentration immediately is 50 grams per liters, and temperature is 90 ℃ a ammonium chloride solution, and the speed of adding guarantees that the filter cake surface does not form be full of cracks, until adding.It is 0.3 that the consumption of ammonium chloride makes the weight ratio of ammonium chloride and molecular sieve, when the absence of liquid of filter cake surface, add temperature immediately and be 90 ℃ deionized water wash filter cake, the consumption of deionized water is 3 times of molecular sieve weight, 120 ℃ of oven dry filter cakes obtain ultra-steady Y molecular sieve Z1.Sodium oxide content is 0.9 weight % among the Z1.
Example 2
Take by weighing Comparative Examples 2 described and hand over a roasting hydrogen Y molecular sieve, the waste liquid A2 that deionized water and Comparative Examples 2 obtain mixes making beating, making molecular sieve content is the slurries that contain molecular sieve of 200 grams per liters, wherein, the consumption of salt (being contained ammonium chloride and sodium-chlor among the used waste liquid A2) is 1.7 weight % of molecular sieve consumption.The molecular sieve pulp that obtains is heated to 90 ℃, pours in the B, simultaneously, filter flask is evacuated to 0.07 MPa, on filter cloth, form the filter cake of about 10 mm thick.When the absence of liquid of filter cake surface, adding concentration immediately is 50 grams per liters, and temperature is 90 ℃ a aqueous ammonium chloride solution.The speed that adds guarantees that the filter cake surface does not form be full of cracks, and it is 0.3 that the ammonium chloride consumption makes the weight ratio of ammonium chloride and molecular sieve.When the absence of liquid of filter cake surface, add temperature immediately and be 90 ℃ deionized water wash filter cake, the consumption of deionized water is 3 times of molecular sieve, and 120 ℃ of oven dry filter cakes obtain Y zeolite Z2, and sodium oxide content is 0.9 weight % among the Z2.
Example 3
(lattice constant is 24.65 dusts, and sodium oxide content is 4.3 weight %, rare earth oxide RE to hand over roasting Rare Earth Y (REY) molecular sieve with one
2O
3Content is 14.2 weight %, wherein, and La
2O
3Content is 4.7 weight %, CeO
2Content is 8.4 weight %, other rare earth oxide contents are 1.1 weight %, Qilu Petrochemical company catalyst plant is produced), deionized water is mixed with into the slurries that contain molecular sieve that molecular sieve content is 150 grams per liters with the waste liquid A1 that Comparative Examples 1 obtains, and the consumption of salt in the slurries (being contained ammonium chloride and sodium-chlor among the used waste liquid A1) is 2.5 weight % of molecular sieve consumption.The slurries that contain molecular sieve that obtain are heated to 60 ℃, pour in the B, simultaneously, filter flask is evacuated to 0.05 MPa, on filter cloth, form the filter cake of about 10 mm thick.When the absence of liquid of filter cake surface, slowly adding concentration immediately is 60 grams per liters, and temperature is 60 ℃ a ammonium sulfate solution.The speed that adds guarantees that the filter cake surface does not form be full of cracks, making the weight ratio of ammonium sulfate and molecular sieve until the consumption of ammonium sulfate is 0.4, when the absence of liquid of filter cake surface, add temperature immediately and be 60 ℃ deionized water wash filter cake, the consumption of deionized water is 4 times of molecular sieve, 120 ℃ of oven dry filter cakes obtain Y zeolite Z3, and sodium oxide content is 1.0 weight % among the Z3.
Example 4
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 ultra-steady Y molecular sieve, hydrochloric acid and deionized water in making beating jar 1, to mix making beating Comparative Examples 1 described, obtain containing the molecular sieve pulp of molecular sieve 150 grams per liters, the consumption of hydrochloric acid is 0.5 weight % of molecular sieve consumption.When the amount of the exchange waste liquid that produces in the liquid receiver 8 is enough, with this waste liquid wholly replace hydrochloric acid, the consumption of waste liquid makes that institute's saliniferous amount is 2.2 weight % of molecular sieve consumption in the waste liquid, 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 acid and/or 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 Z4, and sodium oxide content is 0.9 weight % among the Z4.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 (13)
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 susceptor under filter cake formation district and ion-exchange area transition band, washing, blot filter cake, and unload filter cake from transition band, it is characterized in that, described molecular sieve refers to that one hands over a roasting Y zeolite, acid and/or salt have also been added in the described slurries, the consumption of described acid or salt is the 0.1-5 weight % of molecular sieve consumption, the vacuum tightness assurance filter cake surface that described filter cake forms in district's liquid susceptor does not have be full of cracks substantially, at described ion-exchange area, add the solution that contains ammonium ion on filter cake top, contain the concentration of ammonium ion solution, sodium oxide content is not higher than 1.5 weight % in the Y zeolite that the vacuum tightness of consumption and ion-exchange area liquid receiver 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 acid is selected from one or more in water-soluble organic acid and the mineral acid.
4. method according to claim 3 is characterized in that described acid refers to hydrochloric acid, sulfuric acid, nitric acid and/or phosphoric acid.
5. method according to claim 1 is characterized in that described salt refers to one or more in water-soluble salt.
6. method according to claim 5 is characterized in that, described salt is selected from one or more in the soluble salt hydrochlorate, vitriol, nitrate, phosphoric acid salt of ammonium, basic metal, aluminium, iron, rare earth metal.
7. method according to claim 6 is characterized in that, described salt is selected from one or more in the muriate of ammonium chloride, ammonium sulfate, ammonium nitrate, ammonium phosphate, sodium sulfate, sodium-chlor, SODIUMNITRATE and rare earth metal.
8. method according to claim 1 is characterized in that, described acid and/or salt derive from the exchange waste liquid of ion-exchange area.
9. method according to claim 1 is characterized in that, the consumption of described acid and/or salt is the 0.5-3 weight % of molecular sieve consumption.
10. method according to claim 1 is characterized in that, described slurries are 50-90 ℃ with the temperature that contains ammonium ion solution.
11. method according to claim 1 is characterized in that, the content of molecular sieve is the 100-300 grams per liter in the described slurries, and the vacuum tightness that filter cake forms in district's liquid receiver is the 0.01-0.08 MPa.
12. method according to claim 1, it is characterized in that, it is 0.1-0.8 that the described consumption that contains the ammonium ion aqueous solution makes the weight ratio of ammonium salt and molecular sieve, in ammonium salt, the concentration that contains the ammonium ion aqueous solution is the 50-100 grams per liter, and the vacuum tightness in the ion-exchange area liquid receiver is the 0.01-0.08 MPa.
13. method according to claim 12 is characterized in that, it is 0.2-0.6 that the described consumption that contains the ammonium ion aqueous solution makes the weight ratio of ammonium salt and molecular sieve.
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