CN102795636B - A kind of exchange method of modifying reducing sodium oxide content in Y zeolite - Google Patents
A kind of exchange method of modifying reducing sodium oxide content in Y zeolite Download PDFInfo
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Abstract
Invention describes a kind of exchange method of modifying reducing sodium oxide content in Y zeolite, it is characterized in that, the higher Y molecular sieve of Na content is made at 0-5 DEG C, to contact 0.5-3 hour with the organic acid aqueous solution with containing mineral acid, then be separated, wash, dry, obtain the Y zeolite compared with suboxide sodium content; Wherein H
2o: weight ratio=11-18: 1 of molecular sieve.Present method, significantly reducing in the process of sodium oxide content in Y zeolite, completely without ammonium salt, eliminates ammonia and nitrogen pollution problem from source, also significantly lower in the water consumption in Y zeolite exchange process and discharge of wastewater.
Description
Technical field
The present invention relates to a kind of method reducing sodium oxide content in Y zeolite.More precisely, relate to use low-temperature mixed acid to carry out the exchange of molecular sieve, exchange method of modifying with the molecular sieve reducing sodium oxide content in Y zeolite.
Background technology
In catalytic cracking catalyst production process, for wherein higher sodium oxide content, generally use ammonium salt to the Na in catalyzer and the former powder of active component zeolite molecular sieve thereof
+carry out ion-exchange reduce its sodium oxide content and then improve its Catalytic Cracking Performance, such as CN1210034A, CN1065844A, US4,357,265 and US 3,455,842 all disclose the method exchanging sodium oxide in molecular sieve with ammonium salt.Because the sodium oxide in molecular sieve exchanges more difficult, in order to improve Na
+exchange efficiency, often use excessive ammonium salt in exchange process, repeatedly exchange by fresh solution, such as, with ammonium ion, the former powder of NaY molecular sieve is exchanged, once exchange the Na that can make in Y zeolite
2o content drops to about 5.0 % by weight, adopts the method for repeatedly exchange and intermediate calcination, can make the Na in Y zeolite
2o content is down to less than 1%.In the technique adopting ammonium salt repeatedly to exchange NaY molecular sieve, the consumption (by weight) of usual ammonium salt is generally 1.0-2.0 times of exchanged molecular screen primary powder butt weight.But a large amount of uses of ammonium salt, can cause the ammonia-nitrogen content in Catalyst Production sewage to exceed standard, can not directly discharge, need spend a huge sum of money to build sewage deamination apparatus and drop into the maintenance operation expense of great number.
CN100404432C discloses a kind of method reducing ammonia and nitrogen pollution in process of zeolite modification, in process of zeolite modification, with the sodium in potassium compound exchanging zeolite, the method of further zeolite exchange modification is carried out again with ammonium salt, potassium compound additional proportion is the weight ratio of potassium compound/molecular sieve is 0.01 ~ 0.5, temperature of reaction 5 ~ 100 DEG C, 0.1 ~ 6 hour duration of contact.But the method needs with the sodium in potassium compound exchanging zeolite, and then, then exchange further with ammonium salt, as described in that patent, zeolite is moisture porous silicoaluminate, and its structure forms primarily of silicon-oxy tetrahedron, wherein part Si
4+by Al
3+replace, cause negative charge superfluous, therefore have basic metal or alkaline-earth metal isoequilibrium ion in structure, meanwhile, have certain cavity and duct in zeolite framework, determine that it has ion exchange, its ion-exchange order is:
Cs
+＞Rb
+＞K
+＞NH
4 +＞Ba
2+＞Sr
3+＞Na
+＞Ca
2+＞Fe
3+＞Al
3+＞Mg
2+＞Li
+
Visible, K
+exchange capacity strong, can than the Na being easier to be swapped out in zeolite
+but, due to K
+exchange capacity be better than NH
4 +, go further again with ammonium salt to exchange the K exchanging to zeolite and get on
+obviously be more difficult, and exchange the K got on
+need to be exchanged further by follow-up ammonium salt, zeolite just may be used for catalytic cracking.This method is difficult to industrially implement, and needs to exchange with ammonium salt, still there is the problem of ammonia and nitrogen pollution.
Summary of the invention
The object of this invention is to provide a kind of molecular sieve can eliminating sodium oxide content in the reduction Y zeolite of ammonia and nitrogen pollution and exchange method of modifying.
A kind of exchange method of modifying reducing sodium oxide content in Y zeolite provided by the invention, comprises and makes molecular sieve at 0-5 DEG C, contact 0.5-3 hour with the organic acid aqueous solution with containing mineral acid, be then separated; Wherein, with the weighing scale of molecular sieve butt, H
2o: the weight ratio of molecular sieve is 11-18: 1, with contained H in the described aqueous solution
+meter, organic acid concentration is 0.009-0.9mol/L, and the concentration of mineral acid is 0.001-0.1mol/L.
Concrete, molecular sieve of the present invention exchanges method of modifying, molecular sieve is carried out ion exchange reaction with contacting with the organic acid aqueous solution containing mineral acid, makes H
+exchange Na
+, the sodium oxide content in molecular sieve is reduced.Wherein with the weighing scale of molecular sieve butt, H
2o: weight ratio=11-18: 1 of molecular sieve, preferred 11-15: 1.Wherein, described mineral acid is selected from one or more of hydrochloric acid, sulfuric acid, nitric acid and phosphoric acid, preferred hydrochloric acid, sulfuric acid or nitric acid.Described organic acid is selected from one or more of acetic acid, oxalic acid, citric acid and formic acid, preferred oxalic acid, citric acid or formic acid.With contained H
+densitometer, in the aqueous solution, mineral acid and organic acid total mol concentration are 0.01-1.0mol/L.Organic acid concentration is 0.009-0.9mol/L, preferred 0.05-0.6mol/L; The concentration of mineral acid is 0.001-0.1mol/L, preferred 0.01-0.08mol/L.
Molecular sieve provided by the invention exchanges in method of modifying, and molecular sieve is contacted with the organic acid aqueous solution with containing mineral acid, and the temperature controlling contact process is 0-5 DEG C.The described molecular sieve that makes contacts with the organic acid aqueous solution with containing mineral acid, can first prepare containing mineral acid and the organic acid aqueous solution, in contained H+, in the aqueous solution, organic acid concentration is 0.009-0.9mol/L, preferred 0.05-0.6mol/L, the concentration of mineral acid is 0.001-0.1mol/L, preferred 0.01-0.08mol/L; Then the aqueous solution is cooled to 0-5 DEG C, then molecular sieve and this aqueous solution is pulled an oar, the temperature controlling mixing process is 0-5 DEG C, then in 0-5 DEG C, stirs 0.5-3 hour at preferred 1-5 DEG C; Also can be first molecular sieve is mixed with water prepared slarry of pulling an oar, the temperature controlling slurries is 0-5 DEG C, then under stirring, add organic acid and mineral acid in slurries, wherein in acid adding process, control temperature is 0-5 DEG C, and the amount of acid adding makes the concentration of acid in the final solution obtained be: with contained H
+meter, organic acid concentration is 0.009-0.9mol/L, preferred 0.05-0.6mol/L, and the concentration of mineral acid is 0.001-0.1mol/L, preferred 0.01-0.08mol/L.
Molecular sieve of the present invention exchanges in method of modifying, described molecular sieve is the Y zeolite with faujusite structure, exchange before modified at molecular sieve that molecular sieve sodium content is higher, the requirement of subsequent applications can not be met, the former powder of such as NaY molecular sieve, more such as decrease through exchange modification, sodium content but still need the Y zeolite of reduction further.
Described contacts molecular sieve with acid solution, can be that pure molecular sieve is contacted with aqueous solutions of organic acids with containing mineral acid, also can be that the composition containing molecular sieve is contacted with aqueous solutions of organic acids with containing mineral acid, such as, former for Y zeolite higher for sodium content powder be contacted with acid solution with the composition of carrier.
Molecular sieve provided by the invention exchanges in method of modifying, by molecular sieve with contact 0.5-3 hour containing mineral acid with aqueous solutions of organic acids after, be then separated, the washing of the molecular sieve obtained after also can comprising separation, the step of drying.Be separated, washing, drying means know for those skilled in the art, such as described separation can adopt the method for filtration, is separated by the molecular sieve after exchange with mother liquor; Can wash molecular sieve with deionized water; With air drying cabinet heating or drying can be carried out by expansion drying method to molecular sieve.
Adopt molecular sieve of the present invention to exchange method of modifying, once exchange the Na that can make in Y zeolite
2o content drops to about 4.0 % by weight; Repeatedly molecular sieve of the present invention exchanges method of modifying, can make the Na in Y zeolite
2o content is down to less than 1%.
Molecular sieve provided by the invention exchanges method of modifying, significantly reducing in the process of sodium oxide content in Y zeolite, completely without ammonium salt, eliminates ammonia and nitrogen pollution problem from source; Because the weight of adopted water and molecular screen primary powder butt is smaller, also significantly lower in the water consumption in Y zeolite exchange process and discharge of wastewater; The degree of crystallinity of the Y zeolite after being simultaneously also surprised to find that exchange improves.
Embodiment
The following examples will be further described the present invention, but not thereby limiting the invention.
The former powder of Y zeolite used in embodiment and comparative example is produced by catalyzer asphalt in Shenli Refinery of China Petrochemical Industry, wherein Na
2o content is 13.5 heavy %, lattice constant is 2.467nm, relative crystallinity is 87.5%; Chemical reagent used does not indicate especially, and its specification is chemical pure.
In embodiment and comparative example, lattice constant, the relative crystallinity of molecular sieve adopt RIPP145-90 standard method (see volumes such as " Petrochemical Engineering Analysis method " (RIPP test method) Yang Cuiding by x-ray powder diffraction (XRD), Science Press, nineteen ninety publishes) measure; Na
2o content is by x-ray fluorescence spectrometry.
Said H in embodiment and comparative example
2o: the weight ratio of molecular screen primary powder butt is the weight ratio exchanging the higher former dried bean noodles base of Y zeolite of water used and sodium content in solution, the water consumption of molecular sieve clearing house is the tonnage exchanging molecular screen primary powder butt per ton water used, unit represents with " ton water/ton molecular sieve " usually, numerically namely equals H
2o: the weight ratio of molecular screen primary powder butt.Such as, H in liquid is exchanged
2o: the weight ratio of molecular screen primary powder butt is reduced to 18: 1 by 20: 1, then the water consumption that molecular sieve exchanges reduces 2 tons of water/ton molecular sieve.And water consumption reduction by 0.5 ton of water/ton molecular sieve obviously will reduce enterprise's production cost, significantly improve effects usually.
Embodiment 1
Take acetic acid 2.7 grams add appropriate cold water stir make it dissolve after add the hydrochloric acid 8.1 grams that concentration is 36 % by weight, then continue to add solution dilution is made into lower concentration by cold water mixed acid solution to 1000ml, control solution temperature: 3.5 ± 0.5 DEG C, in stirring, add the former dried bean noodles base of Y zeolite 71.4 grams of (H
2o: weight ratio=14 of molecular screen primary powder butt: 1), then in 3.5 ± 0.5 DEG C of stirring reactions 2 hours, then slurry is filtered, filter cake 5 times of deionized water drip washing to the former grain weight amount of Y zeolite, oven dry, obtain low-temperature and low-concentration and mix the sieve sample that acid solution once exchanges, be designated as S1.Its character and exchange water consumption are in table 1.
Embodiment 2
Take oxalic acid 5.67 grams add appropriate cold water stir make it dissolve after add 15.75 grams, the nitric acid that concentration is 20 % by weight, then continue to add solution dilution is made into lower concentration by cold water mixed acid solution to 1000ml, control solution temperature: 4.5 ± 0.5 DEG C, in stirring, add the former dried bean noodles base of Y zeolite 55.6 grams of (H
2o: weight ratio=18 of molecular screen primary powder butt: 1), then in 4.5 ± 0.5 DEG C of stirring reactions 2.5 hours, then slurry is filtered, filter cake 5 times of deionized water drip washing to the former grain weight amount of Y zeolite, oven dry, obtain low-temperature and low-concentration and mix the sieve sample that acid solution once exchanges, be designated as S2.Its character and exchange water consumption are in table 1.
Embodiment 3
Take citric acid 12.8 grams add appropriate cold water stir make it dissolve after add the phosphoric acid 3.27 grams that concentration is 50 % by weight, then continue to add cold water by solution dilution to the mixed acid solution of 1000ml lower concentration, control solution temperature: 1 ± 0.5 DEG C, in stirring, add the former dried bean noodles base of Y zeolite 66.7 grams of (H
2o: weight ratio=15 of molecular screen primary powder butt: 1), then in 1 ± 0.5 DEG C of stirring reaction 3 hours, then slurry is filtered, filter cake 5 times of deionized water drip washing to the former grain weight amount of Y zeolite, oven dry, obtain low-temperature and low-concentration and mix the sieve sample that acid solution once exchanges, be designated as S3.Its character and exchange water consumption are in table 1.
Embodiment 4
Take acetic acid 6.3 grams add appropriate cold water stir make it to dissolve after to add concentration be the phosphoric acid 2.61 grams of 50 % by weight, 1 gram, the nitric acid of 20 % by weight, then continue to add solution dilution is made into lower concentration by cold water mixed acid solution to 1000ml, control solution temperature: 2.5 ± 0.5 DEG C, in stirring, add the former dried bean noodles base of Y zeolite 83.3 grams of (H
2o: weight ratio=12 of molecular screen primary powder butt: 1), then in 2.5 ± 0.5 DEG C of stirring reactions 1 hour, then slurry is filtered, filter cake 5 times of deionized water drip washing to molecular screen primary powder weight, oven dry, obtain low-temperature and low-concentration and mix the sieve sample that acid solution once exchanges, be designated as S4.Its character and exchange water consumption are in table 1.
Embodiment 5
Take oxalic acid 15.12 grams, citric acid 13.44 grams add appropriate cold water stir make it dissolve after add 15.75 grams, the nitric acid that concentration is 20 % by weight, then continue to add solution dilution is made into lower concentration by cold water mixed acid solution to 1000ml, control solution temperature: 1 ± 0.5 DEG C, in stirring, add the former dried bean noodles base of Y zeolite 90.9 grams of (H
2o: weight ratio=11 of molecular screen primary powder butt: 1), then in 1 ± 0.5 DEG C of stirring reaction 0.5 hour, then slurry is filtered, filter cake 5 times of deionized water drip washing to molecular screen primary powder weight, oven dry, obtain low-temperature and low-concentration and mix the sieve sample that acid solution once exchanges, be designated as S5.Its character and exchange water consumption are in table 1.
Routine ammonium salt of comparative example 1 molecular sieve exchanges
The conventional ammonium salt switching method of former powder is sieved, by molecular screen primary powder butt 50 grams and ammonium chloride and water according to NaY: NH according to Chinese patent CN1210034A Middle molecule
4cl: H
2the weight ratio making beating of O=1: 1: 20, the pH value regulating slurries with dilute hydrochloric acid is 3.0, is warming up to 90 DEG C and stirs 1 hour, then filter, filter cake 10 times of deionized water drip washing to molecular screen primary powder butt weight, oven dry, obtain the molecular sieve that a conventional ammonium salt exchanges, be designated as D1.Its character and exchange water consumption are in table 1.
The mixing acid normal temperature of comparative example 2 molecular sieve exchanges
Take acetic acid 2.7 grams add suitable quantity of water stir make it dissolve after add the hydrochloric acid 8.1 grams that concentration is 36 % by weight, then continue to add solution dilution is made into lower concentration by cold water mixed acid solution to 1000ml, solution temperature is warming up to 40 DEG C, adds NaY type molecular screen primary powder butt 66.7 grams of (H in stirring
2o: weight ratio=15 of molecular screen primary powder butt: 1), stirring reaction is continued 2 hours at 40 DEG C, then slurry is filtered, filter cake 5 times of deionized water drip washing to molecular screen primary powder butt weight, oven dry, the lower concentration obtained under non-cryogenic condition mixes the sieve sample that acid solution once exchanges, and is designated as D2.Its character and exchange water consumption are in table 1.
The high concentration phosphorus acid solution of comparative example 3 molecular sieve once exchanges
Take the phosphatase 11 3.07 grams that concentration is 50 % by weight, then add cold water by solution dilution to the phosphoric acid solution of 1000ml higher concentration, stir and control solution temperature: 2 ± 0.5 DEG C, in stirring, adding molecular screen primary powder butt 66.7 grams of (H
2o: weight ratio=15 of molecular screen primary powder butt: 1), continues stirring reaction 3 hours, exchanges disposed slurry and filters, filter cake 5 times of deionized water drip washing to molecular screen primary powder butt weight, oven dry.The sieve sample that the phosphoric acid solution obtaining low temperature higher concentration once exchanges, is designated as D3.Its character and exchange water consumption are in table 1.
The low-temperature and low-concentration phosphoric acid solution of comparative example 4 molecular sieve once exchanges
Take the phosphoric acid 5.88 grams that concentration is 50 % by weight, then add cold water by solution dilution to the phosphoric acid solution of 1000ml low concentration, stir and control solution temperature: 2 ± 0.5 DEG C, in stirring, adding molecular screen primary powder butt 66.7 grams of (H
2o: weight ratio=15 of molecular screen primary powder butt: 1), continues stirring reaction 3 hours, exchanges disposed slurry and filters, filter cake 5 times of deionized water drip washing to molecular screen primary powder butt weight, oven dry.The sieve sample that the phosphoric acid solution obtaining low-temperature and low-concentration once exchanges, is designated as D4.Its character and exchange water consumption are in table 1.
The citric acid solution of the low temperature higher concentration of comparative example 5 molecular sieve once exchanges
Take citric acid 58.24 grams add appropriate cold water stir make it to dissolve after then continue to add cold water by solution dilution to the citric acid solution of 1000ml higher concentration, stir and control solution temperature: 3 ± 0.5 DEG C, in stirring, adding molecular screen primary powder butt 66.7 grams of (H
2o: weight ratio=15 of molecular screen primary powder butt: 1), continues stirring reaction 1 hour, exchanges disposed slurry and filters, filter cake 5 times of deionized water drip washing to molecular screen primary powder butt weight, oven dry.The sieve sample that the citric acid solution obtaining low temperature higher concentration once exchanges, is designated as D5.Its character and exchange water consumption are in table 1.
The low-temperature mixed acid solution of comparative example 6 molecular sieve once exchanges (low water consumption)
Take oxalic acid 15.12 grams, citric acid 13.44 grams add appropriate cold water stir make it dissolve after add 15.75 grams, the nitric acid that concentration is 20 % by weight, then continue to add solution dilution is made into lower concentration by cold water mixed acid solution to 1000ml, control solution temperature: 1 ± 0.5 DEG C, in stirring, add molecular screen primary powder butt 125 grams of (H
2o: weight ratio=8 of molecular screen primary powder butt: 1), then in 1 ± 0.5 DEG C of stirring reaction 0.5 hour, then slurry is filtered, filter cake 5 times of deionized water drip washing to molecular screen primary powder butt weight, oven dry, obtain low-temperature and low-concentration and mix the sieve sample that acid solution once exchanges, be designated as D6.Its character and exchange water consumption are in table 1.
The low-temperature mixed acid solution of comparative example 7 molecular sieve once exchanges (high water consumption)
Take oxalic acid 15.12 grams, citric acid 13.44 grams add appropriate cold water stir make it dissolve after add 15.75 grams, the nitric acid that concentration is 20 % by weight, then continue to add solution dilution is made into lower concentration by cold water mixed acid solution to 1000ml, control solution temperature: 1 ± 0.5 DEG C, in stirring, add molecular screen primary powder butt 50 grams of (H
2o: weight ratio=20 of molecular screen primary powder butt: 1), then in 1 ± 0.5 DEG C of stirring reaction 0.5 hour, then slurry is filtered, filter cake 5 times of deionized water drip washing to molecular screen primary powder weight, oven dry, obtain low-temperature and low-concentration and mix the sieve sample that acid solution once exchanges, be designated as D7.Its character and exchange water consumption are in table 1.
The performance of table 1Y type sieve sample
From table 1, exchange method of modifying of the present invention can once by Na
2the Y zeolite of O content 13.5% exchanges to Na
2below O content 5% is heavy, meet industrial actual needs completely; The unit cell dimension of Y zeolite is constant, and relative crystallinity increases; Ammonia and nitrogen pollution is eliminated from source; Significantly reduce the water consumption in Y zeolite exchange process.
The result of comparative example shows:
(1) sodium oxide content adopting conventional ammonium switching technology under the prerequisite keeping the degree of crystallinity of Y zeolite not be damaged, the former powder of NaY molecular sieve once to be exchanged is reduced to below 5% weight, but, but bring serious ammonia and nitrogen pollution;
(2) mixing acid of non-cryogenic is adopted to exchange, although the sodium oxide content that former for Y zeolite powder once exchanges to be reduced to below 5% weight, the degree of crystallinity of Y zeolite but receives serious destruction;
(3) single organic acid or mineral acid carry out low temperature exchange, under the condition of low concentration, the sodium oxide content of the former powder of Y zeolite can not be made to be reduced to below 5% weight, if acid concentration is higher, although the sodium oxide content of former for Y zeolite powder can be reduced to below 5% weight, but the degree of crystallinity of Y zeolite but receives serious destruction.
(4) reduce and optimize molecular sieve exchange water consumption (H
2o: the weight ratio of molecular screen primary powder butt) very important for the reduction effect of the sodium oxide guaranteed in molecular sieve: in comparative example 6, although water consumption is few, the reduction effect of the sodium oxide of molecular sieve is unsatisfactory; In comparative example 7, the reduction of the sodium oxide of molecular sieve is effective, but water consumption is bigger than normal.
Claims (7)
1. reduce an exchange method of modifying for sodium oxide content in molecular sieve, it is characterized in that, make molecular sieve at 0-5 DEG C, contact 0.5-3 hour with the organic acid aqueous solution with containing mineral acid, be then separated; Wherein, with the weighing scale of molecular sieve butt, H
2o: the weight ratio of molecular sieve is 11-18: 1, with contained H in the described aqueous solution
+meter, organic acid concentration is 0.009-0.9mol/L, and the concentration of mineral acid is 0.001-0.1mol/L, and described molecular sieve is the Y zeolite with faujusite structure.
2. in accordance with the method for claim 1, it is characterized in that, with the weighing scale of molecular sieve butt, H
2o: the weight ratio of molecular sieve is 11-15: 1.
3. in accordance with the method for claim 1, it is characterized in that, with contained H
+meter, in the described aqueous solution, organic acid concentration is 0.05-0.6mol/L, and the concentration of mineral acid is 0.01-0.08mol/L.
4. in accordance with the method for claim 1, it is characterized in that, the described molecular sieve that makes with the method contacted with aqueous solutions of organic acids containing mineral acid is: molecular sieve and water being pulled an oar forms slurries, is then mixed with mineral acid and organic acid by these slurries, and the temperature controlling mixing process is 0-5 DEG C.
5. in accordance with the method for claim 1, it is characterized in that, described in molecular sieve and mineral acid are contacted with aqueous solutions of organic acids method be: by molecular sieve and the aqueous solution containing organic acid and mineral acid at 0-5 DEG C.
6. in accordance with the method for claim 1, it is characterized in that, described organic acid is selected from one or more in acetic acid, oxalic acid, citric acid and formic acid, and described mineral acid is selected from one or more in hydrochloric acid, sulfuric acid, nitric acid and phosphoric acid.
7. in accordance with the method for claim 6, it is characterized in that, described organic acid is selected from one or more in oxalic acid, citric acid and formic acid, and described mineral acid is selected from one or more in hydrochloric acid, sulfuric acid, nitric acid.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85100324A (en) * | 1985-04-01 | 1986-08-06 | 中国石油化工总公司抚顺石油化工研究院 | Distillate Hydrodewaxing catalyst and preparation method thereof |
| CN1417120A (en) * | 2001-10-30 | 2003-05-14 | 中国石油化工股份有限公司 | Filtering process of water slurry of Y-type molecular sieve |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85100324A (en) * | 1985-04-01 | 1986-08-06 | 中国石油化工总公司抚顺石油化工研究院 | Distillate Hydrodewaxing catalyst and preparation method thereof |
| CN1417120A (en) * | 2001-10-30 | 2003-05-14 | 中国石油化工股份有限公司 | Filtering process of water slurry of Y-type molecular sieve |
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