CN1358566A - Adsorbent, its preparation process and use in separating dimethyl benzene - Google Patents
Adsorbent, its preparation process and use in separating dimethyl benzene Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 239000003463 adsorbent Substances 0.000 title claims abstract description 24
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 34
- 239000000843 powder Substances 0.000 claims abstract description 31
- 229910021536 Zeolite Inorganic materials 0.000 claims abstract description 22
- 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 22
- 238000001179 sorption measurement Methods 0.000 claims abstract description 22
- 239000010457 zeolite Substances 0.000 claims abstract description 22
- 239000011148 porous material Substances 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000005342 ion exchange Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000002594 sorbent Substances 0.000 claims description 56
- 238000000034 method Methods 0.000 claims description 25
- 238000005194 fractionation Methods 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 9
- 238000000465 moulding Methods 0.000 claims description 7
- 238000000746 purification Methods 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 4
- 239000013078 crystal Substances 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000005995 Aluminium silicate Substances 0.000 claims description 3
- 230000004913 activation Effects 0.000 claims description 3
- 238000001994 activation Methods 0.000 claims description 3
- 235000012211 aluminium silicate Nutrition 0.000 claims description 3
- 239000010424 alunite Substances 0.000 claims description 3
- 229910052934 alunite Inorganic materials 0.000 claims description 3
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 3
- KPZTWMNLAFDTGF-UHFFFAOYSA-D trialuminum;potassium;hexahydroxide;disulfate Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Al+3].[Al+3].[Al+3].[K+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O KPZTWMNLAFDTGF-UHFFFAOYSA-D 0.000 claims description 3
- 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 2
- 244000275012 Sesbania cannabina Species 0.000 claims description 2
- 229910001413 alkali metal ion Inorganic materials 0.000 claims description 2
- 229910001420 alkaline earth metal ion Inorganic materials 0.000 claims description 2
- 239000004411 aluminium Substances 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 239000000440 bentonite Substances 0.000 claims description 2
- 229910000278 bentonite Inorganic materials 0.000 claims description 2
- 235000019353 potassium silicate Nutrition 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 2
- 238000012546 transfer Methods 0.000 abstract description 7
- 238000000926 separation method Methods 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 4
- 238000009826 distribution Methods 0.000 abstract description 3
- 239000003513 alkali Substances 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract description 2
- 238000005096 rolling process Methods 0.000 abstract description 2
- 238000005507 spraying Methods 0.000 abstract description 2
- 230000003213 activating effect Effects 0.000 abstract 1
- 239000000853 adhesive Substances 0.000 abstract 1
- 230000001070 adhesive effect Effects 0.000 abstract 1
- 238000000227 grinding Methods 0.000 abstract 1
- 238000010298 pulverizing process Methods 0.000 abstract 1
- YNQLUTRBYVCPMQ-UHFFFAOYSA-N Ethylbenzene Chemical compound CCC1=CC=CC=C1 YNQLUTRBYVCPMQ-UHFFFAOYSA-N 0.000 description 10
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 9
- URLKBWYHVLBVBO-UHFFFAOYSA-N Para-Xylene Chemical group CC1=CC=C(C)C=C1 URLKBWYHVLBVBO-UHFFFAOYSA-N 0.000 description 9
- 239000002245 particle Substances 0.000 description 8
- 241001494479 Pecora Species 0.000 description 5
- 235000009508 confectionery Nutrition 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 159000000009 barium salts Chemical class 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002808 molecular sieve Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 3
- DSNHSQKRULAAEI-UHFFFAOYSA-N 1,4-Diethylbenzene Chemical group CCC1=CC=C(CC)C=C1 DSNHSQKRULAAEI-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- BKIMMITUMNQMOS-UHFFFAOYSA-N nonane Chemical compound CCCCCCCCC BKIMMITUMNQMOS-UHFFFAOYSA-N 0.000 description 2
- 239000001103 potassium chloride Substances 0.000 description 2
- 235000011164 potassium chloride Nutrition 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 239000002156 adsorbate Substances 0.000 description 1
- 230000000274 adsorptive effect Effects 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 description 1
- 229940045511 barium chloride Drugs 0.000 description 1
- 229910001626 barium chloride Inorganic materials 0.000 description 1
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 1
- 229910001864 baryta Inorganic materials 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 150000001555 benzenes Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000009969 flowable effect Effects 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000001404 mediated effect Effects 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000000700 radioactive tracer Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 235000014347 soups Nutrition 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 150000003738 xylenes Chemical class 0.000 description 1
Landscapes
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The present invention discloses an adsorbent, its preparation method and application in the separation of dimethyl benzene. Its preparation method incldues the following steps: adopting X-type zeolite raw powder or Y-type zeolite raw powder whose grain size is 0.5-2 micrometer, adhesive and pore-expanding agent, mixing them into dry powder, grinding by adding water or without water, drying, pulverizing to obtain fine powder, feeding the above-mentioned powder material into disk of grnaulating machine, spraying water, rolling and prilling, activating, drying, alkali treatment and ion exchange so as to obtain the adsorbent with specific secondary pore distribution. Said adsorbent is high in adsorption capacity, large in separatino coefficient and quick in dynamic mass transfer rate.
Description
The present invention relates to a kind of sorbent material, its preparation method and the application in separating dimethyl benzene thereof, X type or y-type zeolite sorbent material, its preparation method and the application in separating paraxylene thereof of particularly a kind of alkalimetal ion and/or alkaline-earth metal ions exchange.
P-Xylol is the important source material of synthesizing polyester resin, and what usually obtained by petrochemical process is the mixture of xylene isomer and ethylbenzene.At present, extensively adopt the Parex technology fractionation by adsorption p-Xylol of UOP (UOP).Realize the fractionation by adsorption of this technology, employed sorbent material is one of its key.Chinese invention patent (publication number CN1184702A) discloses a kind of dimethylbenzene and has separated the preparation method who uses spheroidal adsorbent, and the sorbent material intensity of this method preparation is higher.But what this method related to only is the forming method of general sorbent material, does not relate to sorbent material and prepares related process, only is the sorbent material of drying after forming in the patent, and the performance of undeclared its fractionation by adsorption p-Xylol.
In addition, prior art did not report as yet that the intracrystalline pore (claiming secondary pore again) that sorbent material forms distributed to the influence of performance of the adsorbent when moulding.The contriver discovers: the secondary pore that sorbent material forms when moulding does not influence sorbent material and selects absorption C
8Aromatic hydrocarbons, but secondary pore plays an important role to the mass transfer of adsorbate, by the distribution of control secondary pore, guaranteeing sorbent material intensity, loading capacity, optionally simultaneously can improve the sorbent material rate of mass transfer.
The object of the invention is to provide a kind of sorbent material, and this sorbent material has specific secondary pore and distributes.
Another object of the present invention is to provide a kind of preparation of adsorbent method.
A further object of the present invention is described sorbent material is used for fractionation by adsorption dimethylbenzene.
For achieving the above object, the invention provides a kind of sorbent material and preparation method thereof and its application in separating dimethyl benzene with specific secondary pore distribution.
Sorbent material of the present invention is a kind of X type or y-type zeolite sorbent material, and wherein the secondary pore of sorbent material is distributed as:＞300nm 40～50%, and 200～300nm 25～40%, and 100nm～200nm 10～20%,＜100nm1～15%.The secondary pore of sorbent material＞200nm of the present invention distributes more, can improve the rate of mass transfer of sorbent material, thereby improve the adsorption separation performance of sorbent material.Y-type zeolite of the present invention is KY, BaY or KBaY; X type zeolite of the present invention is KX, BaX or KBaX.
Preparation of adsorbent method of the present invention comprises caking agent, expanding agent, X type zeolite powder or the former powder of y-type zeolite is mixed into even dry powder, add water moulding, drying, activation after alkaline purification, ion-exchange, to make described sorbent material, wherein said zeolite powder crystal grain is between 0.5～2 μ m; The raw material weight proportioning is:
Caking agent 2～17%
Expanding agent 0.5～6.5%
The former powder surplus of X type or y-type zeolite.
Caking agent of the present invention is one or more mixtures in kaolin, wilkinite, bentonite, silicon sol, aluminium colloidal sol, the water glass.The consumption of caking agent is preferably 4～10% of raw material gross weight.And the quality of binding agent also will be controlled, Fe in the caking agent
2O
3＜1% (weight), alunite＜2.5% (weight).In above-mentioned scope, p-Xylol slightly reduces the separation factor of other component on the sorbent material, but whole separation is not had obvious influence.Exceed above-mentioned scope, p-Xylol descends significantly to the separation factor of other component, will have a strong impact on the fractionation by adsorption effect of system.Non-conformity of quality as binding agent closes requirement, and available chemistry or physical method are with Fe
2O
3Or the content of alunite is reduced to span of control, also the product in replaceable satisfactory other place of production.
Expanding agent of the present invention is one or more mixtures in xylogen, sodium cellulosate, the sesbania powder.The expanding agent consumption is preferably 1～4% of raw material gross weight.
The shape of sorbent material of the present invention is sphere or bar shaped preferably, also can be other shape, as particulate state, sheet.Adopt conventional forming method to get final product, as X type zeolite or y-type zeolite, binding agent and expanding agent are mediated extruded moulding by the even back of required mixed water as roll shaping or extrusion.Perhaps raw material is mixed the back water and spray, the rolling balling shape while spraying, 20～60 rev/mins of kinds of control velocity of rotation, 45～60 ° of corners, screening meets the requirements as 20～50 purpose ball-type molecular sieves, and is dry then, and in 300～600 ℃ of roastings.Also available other manufacturing process is as pressed disc method.
Alkali treatment method of the present invention can adopt the described method of document (Yuan in the amber Yanshan Petrochemical, 2 (1992,78)).Used alkaline purification liquid is formed with the used colloidal sol composition of synthesis of molecular sieve similar, to add Al in the caking agent
2O
3Amount is benchmark, preparation crystallization molecular sieve mother liquor, and silica alumina ratio 1～3, sodium-silicon-rate 0.2～1.0, water silicon is than 10～180.90～100 ℃ of temperature, solid-to-liquid ratio 1/1～1/4,6～12 hours treatment times.After the alkaline purification, can adopt ordinary method to carry out ion-exchange, exchange with sylvite or barium salt solution as the zeolite with gained after the alkaline purification, flush away negatively charged ion after drying promptly gets KY, KX or BaX, BaY type sorbent material; Also can select the potassium salt soln exchange for use, and then use barium salt solution exchange system to get KBaX or KBaX sorbent material; Also can adopt the pillar ion-exchange techniques: during as preparation BaX or BaX type sorbent material, control Ba
2+Concentration is 0.1～0.5N, air speed 0.5～4h
-1, 90～100 ℃ of temperature, make the dimethylbenzene fractionation by adsorption with BaX or BaY sorbent material through ion-exchange at 30～90 hours swap times.Also can introduce second metal ion such as K
+Deng, make KBaX or KBaY etc.The described sylvite of ion-exchange or the soluble salt that barium salt is selected from K, Ba of being used for, preferred Repone K, bariumchloride, nitrate of baryta.
Preparation of adsorbent method of the present invention also can also can carefully be handled the back oven dry through adding water mill before adding the water moulding, be ground into powder.As mixed powder being added suitable quantity of water, be mixed into the glutinous shape thing of certain viscosity, ground 1～4 hour through colloidal mill, oven dry is ground into powder then.The add-on of water does not need strict control, as long as help levigately, is 10～40% of raw material dry powder gross weight as controlling amount of water.Through the levigate sorbent material of handling the back preparation, its fractionation by adsorption coefficient ratio is big without the fractionation by adsorption coefficient of the sorbent material of levigate Processing of Preparation, has improved the selectivity of p-Xylol to ethylbenzene, therefore, when preparation separates the sorbent material of the xylene mixture that contains ethylbenzene, preferably pass through levigate processing.
Sorbent material of the present invention is used for fractionation by adsorption dimethylbenzene, is particularly suitable for from xylol or contains fractionation by adsorption p-Xylol the xylol of ethylbenzene.
Accompanying drawing is preparation method's synoptic diagram of the present invention, is one of them preferred version.
Granularity, caking agent quality and content by controlling used zeolite powder, the content of expanding agent can make big, the dynamic fast sorbent material of rate of mass transfer of loading capacity height, separation factor, meet the industrialization sorbent material three primary conditions that must possess.
The present invention is described further below in conjunction with embodiment, but do not limit to its scope.
Intensity described in the following embodiment adopts the granule strength determinator to measure, and getting 30 sorbent material bead strength detection mean values is intensity measurements; Described benzene adsorptive capacity adopts flow method to measure, and the benzene specific pressure is 0.1, and adsorption temp is 35 ± 1 ℃, 550 ℃ of activation 2 hours, dry cooling was put into the saturated benzene vapor that airtight adsorption tank absorption is brought into by nitrogen with the sample of weighing with sorbent material, balance 4 hours is calculated phenenyl absorbing amount according to its weightening finish; Secondary pore distributes and adopts mercury penetration method to measure; 30 zeolite grains are randomly drawed in employing from stereoscan photograph, its globule size mean value is crystal particle diameter.
Implement sharp 1
5.5kg kaolin, 0.5kg xylogen and the former powder 44kg of crystal grain 0.82 μ mX type mix, water spray rotates balling-up, 120 ℃ of oven dry, 550 ℃ of roastings 5 hours, alkaline purification (water silicon is than 100 for silica alumina ratio 2.5, sodium-silicon-rate 1.0), ion-exchange Ba
2+(air speed 2/hr, 90 ℃ of temperature, BaCl
2Strength of solution 0.2N, exchange 40hr), make the BaX sorbent material.Its intensity is measured with the granule strength instrument, adopts the dynamic flow method to measure the sorbent material benzene adsorption capacity, as the index of estimating the adsorbents adsorb capacity.
Fractionation by adsorption coefficients by using pulse dynamic testing evaluation method, adsorption column column length 137cm, sorbent material loadings 70ml.The absorption raw material consist of to,, o-Xylol, ethylbenzene and each 5% (volume) of tracer agent (positive nonane), all the other 75% (volumes) are desorbing agent.Desorbing agent is p-Diethylbenzene 30% (volume)+normal heptane 70% (volume).177 ℃ of adsorption temps, pressure 0.8MPa, charging flow velocity 1.2ml/min.
At first use the saturated adsorption column of desorbing agent, treat system temperature, pressure-stabilisation after, switch to stock liquid pulse sample introduction 10min, after sample introduction finishes, switch back desorbing agent with speed.Take a sample at regular intervals once at the spout place, the concentration of sample was mapped to elution time or volume, obtain sample concentration time changing curve.The peak width at half height of each curve characterizes the dynamic mass transfer speed degree of fractionation by adsorption material, and the ratio of component A, B net retention volume is defined as the fractionation by adsorption factor beta of A, B two components
A/Bβ
A/BBe worth greatly more, show that the separating effect between A, B two components is good more.Concrete evaluating data sees Table 1.Prepared sorbent material secondary pore distributes as follows:＞300nm 42.5%, 200～300nm 28.1%, 100～200nm 15.3%,＜100nm 14.1%.
Table 1 sorbent material evaluating data embodiment intensity phenenyl absorbing amount selectivity rate of mass transfer
A gram/milligram/gram β
Px/ebβ
Px/mxβ
Px/oxMl
Grain 1 286 181 1.94 2.82 2.76 11.9 2 278 179 1.91 2.77 2.81 12.2 3 280 165 1.96 2.66 2.48 12.6 4 156 192 1.96 2.81 2.76 10.3 5 234 189 1.84 2.95 2.86 11.4 6 241 199 2.04 2.97 3.10 9.9 Comparative Examples 1 228 133 1.82 2.96 2.46 11.6 Comparative Examples 2 252 181 1.81 2.86 2.69 16.3
Embodiment 2
The former powder particles of used faujusite Y is 1.4 μ m, and all the other conditions are with embodiment 1, and the performance of the adsorbent evaluating data of preparation sees Table 1.Prepared sorbent material secondary pore distributes as follows:＞300nm 43.6%, 200～300nm 30.1%, 100～200nm 12.8%,＜100nm 13.5%.
Embodiment 3
The former powder particles degree of used faujusite X is 1.12 μ m, the sweet soil of caking agent sheep (place of production: Shanxi, down together) 17%, all the other conditions are with embodiment 1, and the performance of the adsorbent evaluating data of preparation sees Table 1.Prepared sorbent material secondary pore distributes as follows:＞300nm 44.5%, 200～300nm 26.1%, 100～200nm18.7%,＜100nm 10.7%.
Embodiment 4
The former powder particles degree of used faujusite X is 1.12 μ m, and the caking agent sheep is sweet native 4%, and all the other conditions are with embodiment 1, and the performance of the adsorbent evaluating data of preparation sees Table 1.Prepared sorbent material secondary pore distributes as follows:＞300nm 41.8%, 200～300nm 25.4%, 100～200nm 18.5%,＜100nm 14.3%.
Embodiment 5
The former powder particles degree of used faujusite X is 1.12 μ m, and the caking agent sheep is sweet native 7%, and all the other conditions are with embodiment 1, and the performance of the adsorbent evaluating data of preparation sees Table 1.Prepared sorbent material secondary pore distributes as follows:＞300nm 41.6%, 200～300nm 34.9%, 100～200nm 17.3%,＜100nm 6.2%.
Embodiment 6
The former powder particles degree of used faujusite X is 1.12 μ m, caking agent sheep sweet native 7%, mixing of materials is after the levigate processing (soup compound that the water of adding 30% and mixture are made certain flowable state, slowly add about 5% water in the levigate process again, levigate even to guarantee), all the other conditions are with embodiment 1, and the performance of the adsorbent evaluating data of preparation sees Table 1.Prepared sorbent material secondary pore distributes as follows:＞300nm 46.6%, 200～300nm 35.9%, 100～200nm 13.3%,＜100nm 4.2%.
Comparative Examples 1
The former powder particles of used faujusite X is 10.2 μ m, and all the other conditions are with embodiment 6, and the performance of the adsorbent evaluating data of preparation sees Table 1.Prepared sorbent material secondary pore distributes as follows:＞300nm 46.8%, 200～300nm 34.7%, 100～200nm 12.9%,＜100nm 5.6%.
Comparative Examples 2
The former powder particles degree of used faujusite X is 1.12 μ m, and the caking agent sheep is sweet native 7%, does not add expanding agent, and all the other conditions are with embodiment 6, and the performance of the adsorbent evaluating data of preparation sees Table 1.Prepared sorbent material secondary pore distributes as follows:＞300nm 13.2%, 200～300nm 30.9%, 100～200nm 37.3%,＜100nm 18.6%.
Claims (12)
1, the X type or the y-type zeolite sorbent material of the exchange of a kind of alkalimetal ion and/or alkaline-earth metal ions, the secondary pore that it is characterized in that sorbent material is distributed as:＞300nm 40～50% (volume percent), 200～300nm 25～40% (volume percent), 100nm～200nm 10～20% (volume percent),＜100nm 1～15% (volume percent).
2, sorbent material according to claim 1 is characterized in that described y-type zeolite is KY, BaY or KBaY.
3, sorbent material according to claim 1 is characterized in that described X type zeolite is KX, BaX or KBaX.
4, each described preparation of adsorbent method of claim 1～3, comprise caking agent, expanding agent, X type zeolite powder or the former powder of y-type zeolite are mixed into even dry powder, add water moulding, drying, activation after alkaline purification, ion-exchange, to make described sorbent material, it is characterized in that described zeolite powder crystal grain is between 0.5～2 μ m; The raw material weight proportioning is:
Caking agent 2～17%
Expanding agent 0.5～6.5%
The former powder surplus of X type or y-type zeolite.
5, preparation of adsorbent method according to claim 4 is characterized in that described caking agent is one or more mixtures in kaolin, wilkinite, bentonite, silicon sol, aluminium colloidal sol, the water glass.
6, preparation of adsorbent method according to claim 5 is characterized in that Fe in the described caking agent
2O
3＜1% (weight), alunite＜2.5% (weight).
7, preparation of adsorbent method according to claim 4, the consumption that it is characterized in that described caking agent is 4～10% of a raw material gross weight.
8, preparation of adsorbent method according to claim 4, used expanding agent are one or more mixtures in xylogen, sodium cellulosate, the sesbania powder.
9, according to claim 1, the expanding agent consumption is 1～4% of a raw material gross weight.
10, according to each described preparation of adsorbent method of claim 4～8, it is characterized in that before adding the water moulding, also can carefully handling the back oven dry through adding water mill, be ground into powder.
11, preparation of adsorbent method according to claim 10 is characterized in that amount of water is 10～40% of a dry powder gross weight.
12, each described sorbent material of claim 1～3 is used for fractionation by adsorption dimethylbenzene.
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