CN108203100A - Method for improving filtering speed of Y-type molecular sieve - Google Patents
Method for improving filtering speed of Y-type molecular sieve Download PDFInfo
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- CN108203100A CN108203100A CN201611186898.1A CN201611186898A CN108203100A CN 108203100 A CN108203100 A CN 108203100A CN 201611186898 A CN201611186898 A CN 201611186898A CN 108203100 A CN108203100 A CN 108203100A
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- molecular sieve
- type molecular
- sieve
- type
- zeolite
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- 239000002808 molecular sieve Substances 0.000 title claims abstract description 198
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 title claims abstract description 188
- 238000001914 filtration Methods 0.000 title claims abstract description 61
- 238000000034 method Methods 0.000 title claims abstract description 60
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910021536 Zeolite Inorganic materials 0.000 claims abstract description 25
- 239000010457 zeolite Substances 0.000 claims abstract description 25
- 239000002002 slurry Substances 0.000 claims abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 26
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 18
- 239000011734 sodium Substances 0.000 claims description 18
- 229910052708 sodium Inorganic materials 0.000 claims description 18
- 239000000377 silicon dioxide Substances 0.000 claims description 13
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 9
- 239000010936 titanium Substances 0.000 claims description 9
- 229910052719 titanium Inorganic materials 0.000 claims description 9
- 238000005342 ion exchange Methods 0.000 claims description 8
- 238000012986 modification Methods 0.000 claims description 8
- 230000004048 modification Effects 0.000 claims description 8
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 7
- 229910052698 phosphorus Inorganic materials 0.000 claims description 7
- 239000011574 phosphorus Substances 0.000 claims description 7
- 239000010703 silicon Substances 0.000 claims description 7
- 229910052710 silicon Inorganic materials 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 5
- 239000004411 aluminium Substances 0.000 claims description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 5
- 241000269350 Anura Species 0.000 claims description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 3
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 3
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 3
- 229910052788 barium Inorganic materials 0.000 claims description 3
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052796 boron Inorganic materials 0.000 claims description 3
- 229910052791 calcium Inorganic materials 0.000 claims description 3
- 239000011575 calcium Substances 0.000 claims description 3
- 229910052733 gallium Inorganic materials 0.000 claims description 3
- 229910052732 germanium Inorganic materials 0.000 claims description 3
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims description 3
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- 239000011777 magnesium Substances 0.000 claims description 3
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 3
- 229910052712 strontium Inorganic materials 0.000 claims description 3
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 3
- 229910052718 tin Inorganic materials 0.000 claims description 3
- 239000011701 zinc Substances 0.000 claims description 3
- 229910052725 zinc Inorganic materials 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- 229910017119 AlPO Inorganic materials 0.000 claims description 2
- 229910002796 Si–Al Inorganic materials 0.000 claims description 2
- 230000000737 periodic effect Effects 0.000 claims description 2
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 238000005406 washing Methods 0.000 description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 20
- 239000007788 liquid Substances 0.000 description 19
- 239000012065 filter cake Substances 0.000 description 17
- 239000003054 catalyst Substances 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 12
- 238000003756 stirring Methods 0.000 description 11
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 10
- 230000000694 effects Effects 0.000 description 9
- 238000012545 processing Methods 0.000 description 9
- 229910001948 sodium oxide Inorganic materials 0.000 description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 150000003863 ammonium salts Chemical class 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 239000003513 alkali Substances 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 239000003643 water by type Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 235000019270 ammonium chloride Nutrition 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 3
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 3
- 235000011130 ammonium sulphate Nutrition 0.000 description 3
- 238000004523 catalytic cracking Methods 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 230000002939 deleterious effect Effects 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 229910052761 rare earth metal Inorganic materials 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 239000001099 ammonium carbonate Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- -1 organic acid ammonium salt Chemical class 0.000 description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 description 1
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 1
- 239000004254 Ammonium phosphate Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000003483 aging Methods 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 1
- 235000012501 ammonium carbonate Nutrition 0.000 description 1
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 description 1
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 description 1
- 229910000148 ammonium phosphate Inorganic materials 0.000 description 1
- 235000019289 ammonium phosphates Nutrition 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005341 cation exchange Methods 0.000 description 1
- 230000001427 coherent effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 229910000388 diammonium phosphate Inorganic materials 0.000 description 1
- 235000019838 diammonium phosphate Nutrition 0.000 description 1
- 239000002283 diesel fuel Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000012013 faujasite Substances 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 238000002795 fluorescence method Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 1
- 235000019837 monoammonium phosphate Nutrition 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 150000004965 peroxy acids Chemical class 0.000 description 1
- 229920002401 polyacrylamide Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
- C01B39/023—Preparation of physical mixtures or intergrowth products of zeolites chosen from group C01B39/04 or two or more of groups C01B39/14 - C01B39/48
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D37/00—Processes of filtration
- B01D37/02—Precoating the filter medium; Addition of filter aids to the liquid being filtered
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
- C01B39/026—After-treatment
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
A method for improving the filtering speed of a Y-type molecular sieve. The method comprises adding zeolite of non-Y type molecular sieve and/or modified zeolite of non-Y type molecular sieve as filter aid into Y type molecular sieve slurry, mixing, and filtering. The method can obviously improve the filtering speed of the Y-type molecular sieve slurry and is beneficial to the operation of the industrial production process.
Description
Technical field
The present invention relates to a kind of methods for improving molecular sieve filtration speed.
Background technology
Molecular sieve is the active component of catalyst, and different reaction process is catalyzed in catalytic reaction process, wherein, Y types
Molecular sieve has excellent heat and hydrothermal stability, has the characteristics that suitable hole window size and acidity, suitable for petrochemical industry etc.
Process.In synthesis, modifying process in molecular sieve, separation of solid and liquid process is directed to, is related to filtering and the filter efficiency of molecular sieve.
For example, the Y type molecular sieve as catalytic cracking catalyst active component, be first containing silicon, aluminium, sodium alkaline system in close
Into NaY, after filtering, NaY molecular sieve carries out cation exchange drop sodium in the mixed system of the compositions such as ammonium salt, water, using filter,
After the processing such as washing, roasting, the catalytic cracking activity effect of molecular sieve can be just played.Since the particle of molecular sieve is small, molecule
The gel of non-complete crystallization may be contained by sieving in synthetic system, the filter effect and filter efficiency of molecular sieve are directly related to molecule
Can the quality of sieve, the treating capacity and production process that filter is also contributed in industrial processes be smoothed out, therefore,
The filter process of molecular sieve is also that system with molecular sieve for preparing is standby with needing the important link paid close attention in modifying process.
It realizes at present in industrialized solid-liquid separation means, relatively typically using flame filter press or belt type filter
Machine, wherein being filter type more commonly used at present using band filter.
In order to realize effective molecular sieve separation of solid and liquid, Chinese patent CN200480027414.8 and
CN200580014998.X individually discloses a kind of catalyst and preparation method thereof, after the reaction of this method Crystallization of Zeolite, adds in
Flocculant settles molecular sieve, then filters, post-processes, the active component as catalyst prepares catalyst.The flocculation
Agent is polyacrylamide etc., and organic amine flocculant price will also result in environmental pollution.
CN1195677C and CN1195678C individually discloses a kind of filter method of Y type molecular sieve slurries, by Y type molecules
Sieve is beaten the slurries to be formed with water and is placed on the filter cloth of a filter, and liquid is made to pass through filter cloth, wherein, also add in the slurries
Molecular sieve can be improved by having entered acid and/or salt or the mixture that alkali or alkali and salt are also added into the slurries, this method
The rate of filtration, but in molecular sieve pulp add in acid, alkali, salt, if control it is bad may because in slurries local ph it is excessively high or
It is too low, it causes the local failure of molecular sieve structure or increases NH_3-N treating burden；For having been subjected to the molecule of drop sodium processing
Sieve, the sodium content of molecular sieve can be improved using sodium salt, is unfavorable for the performance of molecular sieve active function instead.Chinese patent
CN1261215C discloses a kind of filter method of nano molecular sieve, is addition alkaline medium (such as hydrogen-oxygen in molecular sieve pulp
Change sodium), non-electrolyte (such as ethyl alcohol) and water, improve the rate of filtration of molecular sieve.This method adds in organic solvent, brings subsequent
Processing load；The alkaline mediums such as sodium hydroxide are not suitable for use in the filtering for the molecular sieve for having been subjected to drop sodium processing.
In order to realize effective molecular sieve separation of solid and liquid, ensure the normal operation of filter and production in industrial processes
Process is smoothed out, and despite recent molecular sieve filtration technology, but there is still a need for improve molecular sieve filtration speed, while not
Molecular sieve filtration new technology molecular sieve performance can be adversely affected, environmentally friendly.
Invention content
The object of the present invention is to provide a kind of method of the raising Y type molecular sieve rate of filtration different from existing method, institutes
The method stated does not need to be transformed existing equipment, will not there is deleterious effect, while simple for process, energy to molecular sieve performance
Enough realize the filtering of molecular sieve fast speed, and technology is more environmentally-friendly.
In order to achieve the object of the present invention, the method for the raising Y type molecular sieve rate of filtration described in the method for the present invention, needs
The zeolite filter aid of non-Y type molecular sieve is added in Y type molecular sieve slurries in advance, after being sufficiently mixed, is refiltered.
Specifically, the method disclosed in this invention for improving the Y type molecular sieve rate of filtration, including:It is starched in Y type molecular sieve
Added in liquid non-Y type molecular sieve zeolite and/or by modified non-Y type molecular sieve zeolite as filter aid, after mixing, into
Row filtering, the filter aid is in terms of butt quality, and addition is the 0.2~10% of Y type molecular sieve amount butt quality, preferably
2~6%.
The method disclosed in this invention for improving the Y type molecular sieve rate of filtration, the zeolite of the non-Y type molecular sieve can
To be one or more in Si-Al molecular sieve, phosphorus aluminium profiles molecular sieve, silica zeolite and Titanium Sieve Molecular Sieve.The sial
Type molecular sieve is one or more in X-type, ZSM types and beta-molecular sieve；The phosphorus aluminium profiles molecular sieve be selected from AlPO, SAPO,
It is one or more in MeAPO and MeAPSO molecular sieves；The total silicon molecule is screened from silicalite-1 molecular sieves；It is described
Titanium Sieve Molecular Sieve be selected from TS-1.These molecular sieves are more preferably various forms beta-molecular sieve, various forms SAPO molecular sieve, each
One or more of kind form X-type molecular sieve, various forms ZSM-5 molecular sieve, various forms TS-1 Titanium Sieve Molecular Sieve.
The method disclosed in this invention for improving the Y type molecular sieve rate of filtration, the zeolite of the non-Y type molecular sieve
" various forms " refers to the various forms of molecular sieve, can be H beta-molecular sieves, drop sodium or the β point for not dropping sodium by taking beta-molecular sieve as an example
Any form in son sieve, this is techniques known.
The method disclosed in this invention for improving the Y type molecular sieve rate of filtration, the non-Y type molecular sieve by modification
Zeolite refer to by modifying element is modified, at ion exchange drop at least one of sodium and high-temperature roasting modification mode
Reason.
Specifically, the method disclosed in this invention for improving the Y type molecular sieve rate of filtration, described passes through the non-of modification
The zeolite of Y type molecular sieve refers to the zeolite of non-Y type molecular sieve by modifying element modification, and modifying element is selected from period of element
One or more of III B element, magnesium, calcium, strontium, barium, titanium, zirconium, manganese, zinc, boron, gallium, silicon, germanium, tin, phosphorus in table.The warp
The zeolite for crossing modified non-Y type molecular sieve can also be the molecular sieve that ion exchange drop sodium processing is carried out through peracid and/or ammonium salt,
Wherein acid is selected from ammonium sulfate, ammonium chloride, nitre selected from one or more of hydrochloric acid, sulfuric acid, nitric acid, organic acid, phosphoric acid etc., ammonium salt
One or more of sour ammonium, ammonium phosphate, diammonium hydrogen phosphate, ammonium dihydrogen phosphate, ammonium carbonate, ammonium hydrogen carbonate, organic acid ammonium salt etc..Institute
The zeolite by modified non-Y type molecular sieve stated can also be the molecular sieve handled by high-temperature roasting.Ion exchange drop sodium,
High-temperature roasting is techniques known.
The method disclosed in this invention for improving the Y type molecular sieve rate of filtration, the Y type molecular sieve are various forms of
Y type molecular sieve：Can be the NaY molecular sieve synthesized by crystallization, or NaY molecular sieve drops sodium by ion exchange
Molecular sieve or the element modified Y type molecular sieve of process made from processing and/or high-temperature roasting processing, as long as molecular sieve
In have Y type molecular sieve sial skeleton, faujasite basket structure and silica alumina ratio.The wherein described modifying element changes
Property, ion exchange drop sodium and high-temperature roasting be techniques known.The various forms of Y type molecular sieves typically have
NaY、REY、HY、NH4Y, super steady Y, REHY, REUSY, by element modified Y molecular sieve.It is described it is element modified refer to NaY,
HY、NH4Y, super steady Y, by the periodic table of elements III B element, magnesium, calcium, strontium, barium, titanium, zirconium, manganese, zinc, boron, gallium, silicon,
One or more of germanium, tin, phosphorus are element modified.
The method disclosed in this invention for improving the Y type molecular sieve rate of filtration, in the Y type molecular sieve slurries, Y types point
Son sieve butt solid content is 20~500g/L.
The method disclosed in this invention for improving the Y type molecular sieve rate of filtration, the Y type molecular sieve slurries are in this field
It is filtered under conventional temperature condition, in order to there is better filter effect, it is 5 that the present invention, which recommends the temperature of the molecular sieve pulp,
~90 DEG C.
The method disclosed in this invention for improving the Y type molecular sieve rate of filtration, described is filtered into side commonly used in the art
Formula filters, and filtering is typically completed in filter or funnel.The filter is selected from band filter and flame filter press.
In catalytic reaction process, according to the difference of reaction purpose, more than one molecule is generally required in catalyst composition
Sieve, in catalytic cracking catalyst, usually contains Y type molecular sieve, in order to improve the octane number of catalytically cracked gasoline, catalyst group
Suitable ZSM-5 shape-selective molecular sieves or beta-molecular sieve, therefore, the zeolite drainage as non-Y type molecular sieve may also be contained in
Active component needed for agent and catalyst, will not be to Y using that will not have deleterious effect to the performance of Y type molecular sieve
Type molecular sieve and its processing procedure bring pollution, meanwhile, it may be acted on due to " bridging " of filter aid, between sieve particle
" bridging " influences the coherent condition between sieve particle, so as to influence the rate of filtration of molecular sieve.This additional non-Y types point
The zeolite filter aid particles of son sieve, constituent difference different from the silica alumina ratio of Y type molecular sieve, it is possible to affect Y type molecules
The electronegativity of particle is sieved, so as to the rate of filtration for affecting the electronegativity of Y type molecular sieve system, influencing molecular sieve.
The present invention is directly added into the zeolite filter aid of non-Y type molecular sieve in Y type molecular sieve slurries, does not need to set to existing
It is standby to be transformed, moreover, filter aid can use in itself as the active component of catalyst, do not pollute the environment, it will not be to Y types
Molecular sieve performance has deleterious effect.The zeolite filter aid of non-Y type molecular sieve is added in, the rate of filtration of Y type molecular sieve can be improved,
This method is simple for process, and molecular sieve filtration technology is more environmentally-friendly.
Specific embodiment
Following example is method in order to further illustrate the present invention, but be should not be limited thereto.
(1) experimental method used in embodiment
1. the measure of the rate of filtration：The filter process for the band filter industrially taken and laboratory use Buchner funnel
The filter process principle of progress is identical, and only the filter cloth of belt filter is mobile, and uses the filtered of Buchner funnel
Journey carries out in the original location, and the filtering rule of the two is identical.Experiment is using Buchner funnel Suction filtration device, for experimental data
Comparativity using same Buchner funnel and same vacuum pump, controls same filtering vacuum degree, and use similary weight
Butt meter Y type molecular sieve.
(2) analysis test method used in embodiment
1. sodium oxide content：It is analyzed using X-fluorescence method.
2. the determination of activity of molecular sieve：It is carried out in the CSA-B type catalyst evaluation devices of Huayang company production.Molecular sieve
In advance under 800 DEG C, 100% water vapor conditions after aging 17h, huge port light diesel fuel is used to carry out determination of activity, reaction for raw material
460 DEG C, reaction time 70s, catalyst loading amount 5.0g of temperature, oil ratio 3.2.
(3) raw materials used specification in embodiment
1.NaY molecular sieves (igloss 34.5%), REUSY molecular sieves (RE2O3Content 8.05%, Na2O content 3.89%, warp
Cross a calcination process), super steady Y (Na2O content 4.23%, by a calcination process), nitric acid rare earth (RE2O3Concentration 270g/
L)：It is industrial goods, picks up from Catalyst Factory of Lanzhou Petrochemical Company.
2.SAPO-34 molecular sieves (sodium oxide content 0.15%), low silica ZSM-5 molecular sieve (silica alumina ratio 33, sodium oxide content
0.15%), high silica ZSM-5 molecular sieve (silica alumina ratio is more than 300, sodium oxide content 0.10%), beta-molecular sieve (sodium oxide content
0.12%)：It is purchased from Shanghai brilliance Chemical Industry Science Co., Ltd.
3.X molecular sieves：Shanghai molecular sieve factory produces, sodium oxide content 3.84%.
4. ammonium sulfate, ammonium chloride, ammonium nitrate：It is chemical reagent.
5. hydrochloric acid：Concentration 36%, chemical reagent.Concentrated ammonia liquor：Concentration 25%, chemical reagent.
Embodiment 1
30g NaY molecular sieves (butt) are added in 164mL deionized waters, under stirring, 5.4g ammonium sulfate is added in, uses
Hydrochloric acid adjusts slurry pH value 4.06, stirs 1h, obtains drop sodium treated molecular sieve pulp, adds in 1.61g (butt meter) high silicon
ZSM-5 molecular sieve continues stirring 10 minutes, and obtained molecular sieve pulp is poured into filtering, filtering vacuum degree in Buchner funnel later
Since 0.07 megapascal during the no liquid of filter cake surface, add in 100mL water washings, the timing being initially added into washing water, until filter cake table
Face no liquid exists, and records washing time, be 3 points 40 seconds.According to washing time, it can be determined that the rate of filtration of molecular sieve.
Comparative example 1
Other than 1.61g (butt meter) high silica ZSM-5 molecular sieve will be added without in the molecular sieve pulp in embodiment 1,
Other conditions are with embodiment 1, after Ammonium Salt Ionic exchanges, add in 100mL water washings, the timing since being initially added into washing water, directly
To filter cake surface no liquid exist, record washing time, be 4 points 30 seconds.
Embodiment 2
The super steady Y (butt) of 30g are added in 180mL deionized waters, under stirring, 85 DEG C is heated to, adds in 2.1g nitre
Sour ammonium, 2.2mL nitric acid rare earths stir 1.5h, obtain rare earth modified, drop sodium treated molecular sieve pulp, add 0.62g
(butt meter) low silica ZSM-5 and 2.00g (butt meter) SAPO-34 molecular sieves continue stirring 5 minutes, the molecular sieve that will be obtained later
Slurries pour into Buchner funnel filtering, 0.07 megapascal of filtering vacuum degree, during the no liquid of filter cake surface, add in 100mL water washings, from
Be initially added into washing water and start timing, until filter cake surface no liquid exists, record washing time, be 3 points 20 seconds.
Comparative example 2
In addition to the low silica ZSM-5s of 0.62g (butt meter) and 2.00g (butts will be added without in the molecular sieve pulp in embodiment 2
Meter) except SAPO-34 molecular sieves, other conditions are the same as embodiment 2.Rare earth modified, drop sodium treated the direct mistake of molecular sieve pulp
Since filter during the no liquid of filter cake surface, add in 100mL water washings, the timing being initially added into washing water, until filter cake surface aneroid
Body exist, record washing time, be 4 points 40 seconds.
Embodiment 3
30g REUSY molecular sieves (butt) are added in 210mL deionized waters, under stirring, 80 DEG C is heated to, adds in
3.0g ammonium chlorides stir 0.5h, add in 1.20g (butt meter) beta-molecular sieve and continue to stir 0.5h, the molecule screening the pulp that will be obtained later
Liquid pours into Buchner funnel filtering, 0.07 megapascal of filtering vacuum degree, during the no liquid of filter cake surface, adds in 100mL water washings, from opening
Begin to add in washing water and start timing, until filter cake surface no liquid exists, record washing time, be 3 points 45 seconds.
Comparative example 3
Other than 1.20g (butt meter) beta-molecular sieve will be added without in the molecular sieve pulp in embodiment 3, other conditions
With embodiment 3, after Ammonium Salt Ionic exchanges, 100mL water washings, the timing since being initially added into washing water, until filter cake table are added in
Face no liquid exists, and records washing time, be 4 points 35 seconds.
Comparative example 4
It is replaced in addition to 1.20g (butt meter) beta-molecular sieves will be added without in embodiment 3 with the concentrated ammonia liquor of concentration 25%
Except (dosage of concentrated ammonia liquor makes the 3 weight % that the dosage of ammonia is REUSY molecular sieves), other conditions are the same as embodiment 3, ammonium salt
After ion exchange, 100mL water washings, the timing since being initially added into washing water are added in, until filter cake surface no liquid exists, note
Record washing time, be 3 points 43 seconds.
Embodiment 4
30g NaY molecular sieves (butt) are added in 300mL deionized waters, stirring forms slurries, adds in 0.6g (butts
Meter) X molecular sieve continues stirring 5 minutes, obtained molecular sieve pulp is poured into Buchner funnel filtering, filtering vacuum degree later
Since 0.07 megapascal during the no liquid of filter cake surface, add in 100mL water washings, the timing being initially added into washing water, until filter cake table
Face no liquid exists, and records washing time, be 4 points 20 seconds.
Comparative example 5
According to existing patented technology, molecular sieve pulp directly filters, and is added without solid filter-aids.
Other than 0.6g (butt meter) X molecular sieve will be added without in the molecular sieve pulp in embodiment 4, other conditions are same
Embodiment 4 records washing time, is 5 minutes.
Embodiment 1 and comparative example 1 the experimental results showed that, after adding in high silica ZSM-5 molecular sieve filter aid, the mistake of molecular sieve
The filter time shorten to 3 points for 30 seconds 40 seconds by 4 points, and filtration time shortens 18.5%, illustrates that the rate of filtration significantly improves.
Embodiment 2 and comparative example 2 the experimental results showed that, after adding in low silica ZSM-5 and SAPO-34 molecular sieve filter aids,
The filtration time of molecular sieve shorten to 3 points for 40 seconds 20 seconds by 4 points, and filtration time shortens 28.6%, equally illustrates to add in drainage
After agent, the rate of filtration of molecular sieve pulp significantly improves.
Embodiment 3 and comparative example 3 the experimental results showed that, beta-molecular sieve filter aid is added in REUSY molecular sieve exchange process
Afterwards, the washing filtering time of molecular sieve shorten to 3 points for 35 seconds 45 seconds by 4 points, and filtration time shortens 18.2%, illustrates in molecule
It sieves after adding in filter aid in ion exchange process, the rate of filtration of molecular sieve significantly improves.
Embodiment 3 and comparative example 4 the experimental results showed that, beta-molecular sieve filter aid is added in REUSY molecular sieve pulps or is added
Enter alkali, molecular sieve filtration speed is suitable.
Embodiment 4 and comparative example 5 the experimental results showed that, after adding in X molecular sieve filter aid in NaY molecular sieve slurries, point
The washing filtering time of son sieve shorten to 4 points 20 seconds by 5 minutes, and filtration time shortens 13.3%, illustrates to hand over without ion
It changes in the NaY molecular sieve slurries of processing after adding in filter aid, the rate of filtration of NaY molecular sieve significantly improves.
The molecular sieve filter cake after molecular sieve filter cake and the washing of comparative example 1~5 after Examples 1 to 4 is washed, at 120 DEG C
Drying, carries out analysis test, the results are shown in Table 1.
The property of 1 molecular sieve of table
Table 1 the result shows that, using the method for the present invention carry out Y type molecular sieve slurries filtering, improve molecular sieve filtration speed
While spending, the sodium oxide content of molecular sieve filter cake will not be improved, the activity of molecular sieve will not be reduced.With using comparative example 4
The prior art compare, although the rate of filtration of molecular sieve pulp is suitable, using the molecular sieve filter cake oxidation of the gained of embodiment 3
Sodium content is significantly low, and (sodium oxide molybdena is 0.99 percentage point low, and activity is 12 percentage points high, sees for the apparent height of 17h steam agings activity
Table 1).
Certainly, the present invention can also have other various embodiments, without deviating from the spirit and substance of the present invention, ripe
Various corresponding changes and deformation, but these corresponding changes and deformation can be made according to the present invention by knowing those skilled in the art
It should all belong to the scope of protection of the present invention.
Claims (10)
- A kind of 1. method for improving the Y type molecular sieve rate of filtration, it is characterised in that this method includes：In Y type molecular sieve slurries The zeolite of the zeolite of non-Y type molecular sieve and/or the non-Y type molecular sieve by modification is added in as filter aid, after mixing, was carried out Filter, for the filter aid in terms of butt quality, addition is the 0.2~10% of Y type molecular sieve butt quality.It is preferred that 2~ 6%.
- 2. according to the method described in claim 1, it is characterized in that the zeolite of the non-Y type molecular sieve is sial type molecule It is one or more in sieve, phosphorus aluminium profiles molecular sieve, silica zeolite, Titanium Sieve Molecular Sieve.
- 3. according to the method described in claim 2, it is characterized in that the Si-Al molecular sieve is selected from X-type, ZSM types, beta molecule It is one or more in sieve；One kind in AlPO, SAPO, MeAPO, MeAPSO molecular sieve of the phosphorus aluminium profiles molecular sieve or It is a variety of；The total silicon molecule is screened from silicalite-1 molecular sieves；The Titanium Sieve Molecular Sieve is selected from TS-1.
- 4. according to the method described in claim 2, it is characterized in that the zeolite of the non-Y type molecular sieve is selected from various forms β Molecular sieve, various forms SAPO molecular sieve, various forms X-type molecular sieve, various forms ZSM-5 molecular sieve and various forms TS-1 One or more of Titanium Sieve Molecular Sieve.
- 5. method according to claim 1 or 2, it is characterised in that the zeolite by modified non-Y type molecular sieve Refer to be handled by modifying element modification, ion exchange drop at least one of sodium and high-temperature roasting modification mode.
- 6. according to the method described in claim 5, it is characterized in that the zeolite by modified non-Y type molecular sieve refers to The zeolite of non-Y type molecular sieve pass through modifying element modification, the modifying element in the periodic table of elements III B element, One or more of magnesium, calcium, strontium, barium, titanium, zirconium, manganese, zinc, boron, gallium, silicon, germanium, tin, phosphorus.
- 7. method according to claim 1 or 2, it is characterised in that the Y type molecular sieve is various forms of Y types molecules Sieve；Preferably NaY, REY, HY, super steady Y, REHY, REUSY, by one kind in element modified Y molecular sieve.
- 8. method according to claim 1 or 2, it is characterised in that Y type molecular sieve butt in the Y type molecular sieve slurries Solid content is 20~500g/L.
- 9. according to the method described in claim 1, it is characterized in that the Y type molecular sieve slurry temperature is 5~90 DEG C.
- 10. according to the method described in claim 1, it is characterized in that filtering is completed in filter or funnel.
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| CN102872909A (en) * | 2011-07-13 | 2013-01-16 | 华东师范大学 | Molecular sieve aggregate and its preparation method |
| CN103084204A (en) * | 2011-10-27 | 2013-05-08 | 中国石油化工股份有限公司 | Method for treating slurry containing nanometer beta molecular sieve |
| CN103663486A (en) * | 2012-12-11 | 2014-03-26 | 山东齐鲁华信高科有限公司 | Synthetic method of agglomerate Beta-zeolite |
| CN105381816A (en) * | 2014-09-05 | 2016-03-09 | 北京安耐吉能源工程技术有限公司 | Hydrogenation modification catalyst and applications thereof |
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|---|---|---|---|---|
| CN102872909A (en) * | 2011-07-13 | 2013-01-16 | 华东师范大学 | Molecular sieve aggregate and its preparation method |
| CN103084204A (en) * | 2011-10-27 | 2013-05-08 | 中国石油化工股份有限公司 | Method for treating slurry containing nanometer beta molecular sieve |
| CN103663486A (en) * | 2012-12-11 | 2014-03-26 | 山东齐鲁华信高科有限公司 | Synthetic method of agglomerate Beta-zeolite |
| CN105381816A (en) * | 2014-09-05 | 2016-03-09 | 北京安耐吉能源工程技术有限公司 | Hydrogenation modification catalyst and applications thereof |
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