US20100278723A1 - Zeolite y - Google Patents

Zeolite y Download PDF

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Publication number
US20100278723A1
US20100278723A1 US12/768,969 US76896910A US2010278723A1 US 20100278723 A1 US20100278723 A1 US 20100278723A1 US 76896910 A US76896910 A US 76896910A US 2010278723 A1 US2010278723 A1 US 2010278723A1
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Prior art keywords
zeolite
temperature
bar
partial pressure
steam partial
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Abandoned
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US12/768,969
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English (en)
Inventor
David Allen Cooper
Cornelis Ouwehand
László Domokos
Lay Hwa Ong
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PQ Corp
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Individual
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Priority to US12/768,969 priority Critical patent/US20100278723A1/en
Assigned to PQ CORPORATION reassignment PQ CORPORATION ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: COOPER, DAVID ALLEN, DOMOKOS, LASZLO, ONG, LAY HWA, OUWEHAND, CORNELIS
Publication of US20100278723A1 publication Critical patent/US20100278723A1/en
Assigned to CREDIT SUISSE AG, AS SUCCESSOR AGENT reassignment CREDIT SUISSE AG, AS SUCCESSOR AGENT SECOND LIEN GRANT OF SECURITY INTEREST IN PATENTS AMENDMENT NO. 1 Assignors: PQ CORPORATION
Assigned to CREDIT SUISSE AG, AS SUCCESSOR AGENT reassignment CREDIT SUISSE AG, AS SUCCESSOR AGENT FIRST LIEN GRANT OF SECURITY INTEREST IN PATENTS AMENDMENT NO. 1 Assignors: PQ CORPORATION
Assigned to PQ CORPORATION reassignment PQ CORPORATION RELEASE OF SECURITY INTEREST IN PATENTS Assignors: CREDIT SUISSE AG, CAYMAN ISLANDS BRANCH
Assigned to PQ CORPORATION reassignment PQ CORPORATION RELEASE OF SECURITY INTEREST IN PATENTS Assignors: CREDIT SUISSE AG, CAYMAN ISLANDS BRANCH
Assigned to CREDIT SUISSE AG, CAYMAN ISLANDS BRANCH, AS ADMINISTRATIVE AGENT reassignment CREDIT SUISSE AG, CAYMAN ISLANDS BRANCH, AS ADMINISTRATIVE AGENT SECURITY AGREEMENT Assignors: POTTERS INDUSTRIES, LLC, PQ CORPORATION
Assigned to WILMINGTON TRUST, NATIONAL ASSOCIATION, AS ADMINISTRATIVE AGENT reassignment WILMINGTON TRUST, NATIONAL ASSOCIATION, AS ADMINISTRATIVE AGENT SECURITY AGREEMENT Assignors: POTTERS INDUSTRIES, LLC, PQ CORPORATION
Priority to US14/157,022 priority patent/US9308521B2/en
Assigned to PQ CORPORATION, POTTERS INDUSTRIES, LLC reassignment PQ CORPORATION RELEASE BY SECURED PARTY (SEE DOCUMENT FOR DETAILS). Assignors: WILMINGTON TRUST, NATIONAL ASSOCIATION, AS ADMINISTRATIVE AGENT
Assigned to PQ CORPORATION, POTTERS INDUSTRIES, LLC reassignment PQ CORPORATION RELEASE BY SECURED PARTY (SEE DOCUMENT FOR DETAILS). Assignors: CREDIT SUISSE AG, CAYMAN ISLANDS BRANCH, AS ADMINISTRATIVE AGENT
Abandoned legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/16—Alumino-silicates
    • B01J20/18—Synthetic zeolitic molecular sieves
    • B01J20/186—Chemical treatments in view of modifying the properties of the sieve, e.g. increasing the stability or the activity, also decreasing the activity
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J29/00—Catalysts comprising molecular sieves
    • B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
    • B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
    • B01J29/08—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the faujasite type, e.g. type X or Y
    • B01J29/084—Y-type faujasite
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
    • 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
    • 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
    • C01B39/20—Faujasite type, e.g. type X or Y
    • C01B39/24—Type Y
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00—Purification; Separation; Use of additives
    • C07C7/12—Purification; Separation; Use of additives by adsorption, i.e. purification or separation of hydrocarbons with the aid of solids, e.g. with ion-exchangers
    • C07C7/13—Purification; Separation; Use of additives by adsorption, i.e. purification or separation of hydrocarbons with the aid of solids, e.g. with ion-exchangers by molecular-sieve technique
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/42—Materials comprising a mixture of inorganic materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2229/00—Aspects of molecular sieve catalysts not covered by B01J29/00
    • B01J2229/10—After treatment, characterised by the effect to be obtained
    • B01J2229/16—After treatment, characterised by the effect to be obtained to increase the Si/Al ratio; Dealumination
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2229/00—Aspects of molecular sieve catalysts not covered by B01J29/00
    • B01J2229/30—After treatment, characterised by the means used
    • B01J2229/36—Steaming

Definitions

  • the present invention relates to modified zeolite Y and to a process for preparing such zeolite Y.
  • Zeolite Y is a well-known zeolite form and has a wide range of documented uses as catalyst supports, adsorbents, selective separation materials, etc. in the petrochemical and chemical industries and also as pollution control materials for industrial, domestic and automotive use.
  • Zeolite Y for example, is one of the main zeolitic materials proposed for hydrocracking use.
  • the present invention provides a process for preparing a zeolite Y having a silica to alumina molar ratio of at least 10 to calcination at a temperature of from 700 to 1000° C. wherein (i) the steam partial pressure is at most 0.06 bar at a temperature of from 700 to 800° C., (ii) the steam partial pressure is at most 0.08 bar at a temperature of from 800 to 850° C., (iii) the steam partial pressure is at least 0.03 bar at a temperature of from 850 to 900° C., and (iv) the steam partial pressure is at least 0.05 bar at a temperature of from 900 to 950° C. and (v) the steam partial pressure is at least 0.07 bar at a temperature of from 950 to 1000° C. Furthermore, the present invention relates to zeolite Y obtainable by such process.
  • the present invention further relates to zeolite Y having a silica to alumina molar ratio of at least 10, the infrared spectrum of which carrier has a peak at 3700 cm ⁇ 1 but substantially no peak at 3670 cm ⁇ 1 .
  • the present invention also relates to zeolite Y having a silica to alumina molar ratio of at least 10, which carrier has an acidity as measured by exchange with perdeuterated benzene of at most 20 micromole/gram.
  • the calcination of the zeolite Y is carried out at a temperature of from 700 to 1000° C.
  • the time during which the zeolite Y is calcined influences the exact temperature to be applied. Generally, the temperature is at most 850° C. At a calcination temperature of more than 900° C., loss of crystallinity was observed.
  • the time during which the zeolite Y is calcined preferably is of from 20 minutes to 5 hours, more preferably of from 30 minutes to 4 hours.
  • the time period to be applied depends on whether the oven is preheated or whether the temperature is increased while the catalyst carrier is being calcined.
  • the time period preferably is at least 40 minutes, more preferably at least 50 minutes. Further, the time period is preferably less than 4 hours, more preferably less than 3 1 ⁇ 2hours.
  • the temperature preferably is at most 850° C., more preferably at most 820° C., most preferably at most 800° C.
  • the calcination can be carried out in the presence or in the absence of steam dependent on the temperature applied.
  • the steam partial pressure preferably is at most 0.04 bar at a temperature of from 700 to 800° C.
  • the steam partial pressure preferably is at most 0.07 bar at a temperature of from 800 to 850° C.
  • the steam partial pressure preferably is at least 0.05 bar, more specifically at least 0.07 bar at a temperature of from 850 to 900° C.
  • the steam partial pressure preferably is at least 0.07 bar at a temperature of from 900 to 950° C.
  • the steam partial pressure preferably is at least 0.08 bar, more specifically at least 0.1 at a temperature of from 950 to 1000° C. If steam is present, the steam partial pressure preferably is at most 0.5 bar, more specifically at most 0.4 bar.
  • the zeolite Y is calcined in the absence of amorphous binder.
  • Preferred zeolite Y materials for use in the present invention are zeolite Y having a silica to alumina ratio (SAR) of more than 10, especially an ultrastable zeolite Y (USY) or a very ultrastable zeolite Y (VUSY) of unit cell size (a o ) less than 2.440 nm (24.40 ⁇ ), in particular less than 2.435 nm (24.35 ⁇ ) and a SAR of more than 10, specifically of more than 10 up to 100.
  • Suitable zeolite Y materials are known, for example, from European Patent Specifications Nos. 247 678 and 247 679, and WO 2004/047988.
  • Preferred VUSY zeolite of EP-A-247 678 or EP-A-247 679 is characterised by a unit cell size below 2.445 nm (24.45 ⁇ ) or 2.435 nm (24.35 ⁇ ), a water adsorption capacity (at 25° C. and a p/p o value of 0.2) of at least 8% wt of the zeolite and a pore volume of at least 0.25 ml/g wherein between 10% and 60% of the total pore volume is made up of pores having a diameter of at least 8 nm.
  • zeolite Y materials described in WO-A-2004/050548.
  • Such materials can be described as a zeolite Y having a SAR of greater than 13, a unit cell size in the range of from 24.10 to 24.40 ⁇ , and a surface area of at least 875 m 2 /g as measured by the BET method and ATSM D 4365-95 with nitrogen adsorption at a p/p o values of 0.02, 0.03 and 0.04.
  • Said materials can be prepared by a process which comprises
  • unit cell size in the range of from 24.14 to 24.38, preferably from 24.24, more preferably from 24.30, to 24.38, preferably to 24.36, especially to 24.35 ⁇ , and specifically in the range of from 24.14 to 24.33 ⁇ ; a SAR in the range of from 20 to 100, preferably from 20 to 80, especially to 50; surface area of at least 890, specifically at least 910 m 2 /g; a micropore volume, as determined by nitrogen porosimetry using the t-plot method, also known as the t-method, using nitrogen as the adsorbate as described by Lippens, Linsen and de Boer, Journal of Catalysis, 3-32,(1964), of greater than 0.28 ml/g, suitably greater than 0.30 ml/g. Generally micropore volume will be less than 0.40 ml/g, suitably less than 0.35 ml/g.
  • micropores are pores having a diameter of less than
  • the present invention also relates to zeolite Y according to the present invention having an acidity as measured by exchange with perdeuterated benzene of at most 20 micromole/gram.
  • This acidity more preferably is at most 15, more preferably at most 12, more preferably at most 10 and most preferably at most 8 micromole/gram.
  • the zeolites of the present invention find particular use as adsorbents, showing versatility in the type of material that can be absorbed. Adsorption capability even at low partial pressure of adsorbate has been found for both polar and non-polar materials. This makes the zeolites of the present invention very attractive for general adsorbency use and for use in pollution control.
  • polar materials water and polar hydrocarbons may be mentioned.
  • mon-polar materials non-polar hydrocarbons, such as aromatic hydrocarbons, for example benzene and toluene, may be mentioned.
  • the present invention also provides for use as adsorbents of the modified zeolites Y according to the present invention, especially the zeolites Y of reduced acidity.
  • Unit cell size Determined by X-ray diffraction using the method of ASTM D-3942-80.
  • Surface Area Determined in accordance with the conventional BET (Brunauer-Emmett-Teller) method nitrogen adsorption technique as described in the literature at S. Brunauer, P. Emmett and E. Teller, J. Am. Chm. Soc., 60, 309 (1938), and ASTM method D4365-95. In the determinations quoted below, the results are given as a single point assessment taken at a nitrogen partial pressure of 0.03 following a high temperature pretreatment. (see also note below).
  • the zeolite Y utilised in the catalysts of the present invention was prepared in accordance with the teaching of WO 2004/047988.
  • the starting material used was low alkali content ( ⁇ 1.5% wt alkali oxide) ammonium form Y zeolites.
  • These zeolites were prepared by one of two methods known in the art. While not meaning to be exclusive of other methods of achieving similar results, the examples were prepared by either the Cooper method (as described in U.S. Pat. No. 5,435,987) which involves K ion exchange of Na form zeolite Y, followed by ammonium ion exchange, or by the Alafandi method (as described in U.S. Pat. No.
  • the zeolite Y obtained had a silica to alumina molar ratio of 25, a unit cell size of 24.33 A and a surface area of 922 m 2 /g.
  • the IR spectrums of the above catalyst carriers were measured with the help of a Biorad FTS 175 FT-IR spectrometer using a mercury cadmium telluride detector.
  • the cell is equipped with a sample holder comprising 10 positions and samples have been measured as self-supporting wafers with a diameter of 18 mm, pressed from 25.3+/ ⁇ 0.1 mg zeolite powder at 3.5-4 Ton pressure.
  • For the background measurement an open position of the sample holder has been used. Background and sample spectra have been measured by collecting 250 scans at 2 cm ⁇ 1 resolution.
  • the spectrometer is flushed with nitrogen to minimize the interference of water vapor.
  • samples After evacuating to less than 5 ⁇ 10 ⁇ 4 mbar, samples have been activated in situ in a special heating zone by applying a temperature program of ramping to 450° C. at a rate of 10° C./min, with a hold time of 30 minutes at 450° C. Subsequently, samples have been cooled to 50° C. with 20° C./min. Then background and sample IR spectra have been measured.
  • the sample holder is slided back to the heating zone, and equilibrated at 50° C. for an additional 15 min, while the vacuum is maintained.
  • H/D exchange has been performed in situ by letting 8-9 Ton of hexadeuterobenzene (C 6 D 6 ) interact with the activated zeolite samples for 15 min at 50° C. followed by evacuation for 45 minutes to a target pressure of 5 ⁇ 10 ⁇ 4 mbar (with a maximum of 1 hour). Then background and sample IR spectra have been measured.
  • the IR spectra of the sample before (OH spectrum) and after (OD spectrum) contact with hexadeuterobenzene were compared as follows. The obtained OH spectrum was subtracted from the OD spectrum and baseline corrected. Then curve-fitting was performed with a predefined peak set for VUSY type materials and previously determined extinction coefficients.
  • the crystallinity is measured by comparing with a highly crystalline VUSY reference by following the changes in peak broadening measured by XRD.
  • Table 1 shows the properties of a sample of zeolite Y prepared as described above which has been calcined for 2 hours at 600° C.
  • Table 3 shows the properties of a sample of zeolite Y prepared as described above and having been calcined for 2 hours at 600° C.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Water Supply & Treatment (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)
  • Catalysts (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
US12/768,969 2009-04-29 2010-04-28 Zeolite y Abandoned US20100278723A1 (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
US12/768,969 US20100278723A1 (en) 2009-04-29 2010-04-28 Zeolite y
US14/157,022 US9308521B2 (en) 2009-04-29 2014-01-16 Zeolite Y

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US17369809P 2009-04-29 2009-04-29
US12/768,969 US20100278723A1 (en) 2009-04-29 2010-04-28 Zeolite y

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US14/157,022 Continuation US9308521B2 (en) 2009-04-29 2014-01-16 Zeolite Y

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US14/157,022 Active 2031-03-16 US9308521B2 (en) 2009-04-29 2014-01-16 Zeolite Y

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US (2) US20100278723A1 (cg-RX-API-DMAC7.html)
EP (1) EP2424661B1 (cg-RX-API-DMAC7.html)
JP (2) JP5868314B2 (cg-RX-API-DMAC7.html)
KR (1) KR101728563B1 (cg-RX-API-DMAC7.html)
CN (2) CN102413929A (cg-RX-API-DMAC7.html)
BR (1) BRPI1014350B1 (cg-RX-API-DMAC7.html)
CA (1) CA2760181C (cg-RX-API-DMAC7.html)
DK (1) DK2424661T3 (cg-RX-API-DMAC7.html)
RU (1) RU2487756C1 (cg-RX-API-DMAC7.html)
SG (1) SG175067A1 (cg-RX-API-DMAC7.html)
UA (1) UA99993C2 (cg-RX-API-DMAC7.html)
WO (1) WO2010126955A1 (cg-RX-API-DMAC7.html)
ZA (1) ZA201106589B (cg-RX-API-DMAC7.html)

Families Citing this family (2)

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Publication number Priority date Publication date Assignee Title
IN2014CN04670A (cg-RX-API-DMAC7.html) 2011-12-23 2015-09-18 Shell Int Research
AU2014253496B2 (en) * 2013-10-22 2018-10-18 China Petroleum & Chemical Corporation A metal modified Y zeolite, its preparation and use

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US6284218B1 (en) * 1998-09-23 2001-09-04 Indian Oil Corporation Limited Process for preparing an hydrothermally stable, large crystallite sized, highly crystallite sized, highly crystalline synthetic faujasite zeolite
US20040138051A1 (en) * 1999-09-07 2004-07-15 Zhiping Shan Novel zeolite composite, method for making and catalytic application thereof
US7192900B2 (en) * 2002-11-27 2007-03-20 Shell Oil Company Hydrocracking catalyst
US20110251049A1 (en) * 2005-09-12 2011-10-13 Petroleum Energy Center Method for manufacturing zeolite Y with aluminum and titanium inserted therein
US20080183025A1 (en) * 2007-01-26 2008-07-31 Albemarle Netherlands B.V. Alkylation Process Using A Catalyst Comprising Rare Earth Containing Zeolites And A Hydrogenation Metal

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EP2424661A4 (en) 2014-01-22
ZA201106589B (en) 2012-11-28
JP2015172000A (ja) 2015-10-01
SG175067A1 (en) 2011-11-28
DK2424661T3 (da) 2021-03-08
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