RU2012144456A - METHOD FOR PRODUCING A ZEOLITE ADSORBENT AND A ZEOLITE ADSORBENT - Google Patents

METHOD FOR PRODUCING A ZEOLITE ADSORBENT AND A ZEOLITE ADSORBENT Download PDF

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RU2012144456A
RU2012144456A RU2012144456/05A RU2012144456A RU2012144456A RU 2012144456 A RU2012144456 A RU 2012144456A RU 2012144456/05 A RU2012144456/05 A RU 2012144456/05A RU 2012144456 A RU2012144456 A RU 2012144456A RU 2012144456 A RU2012144456 A RU 2012144456A
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chloride
copper
solution
zeolite
concentrations
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RU2012144456/05A
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Илья Сергеевич Фастов
Сергей Анатольевич Фастов
Владимир Алексеевич Глухов
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Закрытое акционерное общество "Молекулярные технологии и новые материалы"
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Priority to RU2012144456/05A priority Critical patent/RU2012144456A/en
Priority to PCT/RU2013/000933 priority patent/WO2014062099A1/en
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    • 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
    • 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
    • B01J20/3071—Washing or leaching
    • 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
    • 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
    • B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3202—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the carrier, support or substrate used for impregnation or coating
    • B01J20/3204—Inorganic carriers, supports or substrates
    • 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
    • B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3231—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the coating or impregnating layer
    • B01J20/3234—Inorganic material layers
    • B01J20/3236—Inorganic material layers containing metal, other than zeolites, e.g. oxides, hydroxides, sulphides or salts
    • 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
    • C01B39/14—Type A

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Analytical Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Geology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Thermal Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

1. Способ получения цеолитного адсорбента, включающий модифицирование в растворе ионами металлов цеолита типа А, сушку, прокалку, отличающийся тем, что модифицирование осуществляют в растворе при массовом соотношении жидкая фаза:твердая фаза, равном 2,0-20,0, процесс модифицирования в вышеупомянутом растворе проводят при температуре 20-90°С, затем промывают, сушат и прокаливают при температуре 120-550°С.2. Способ по п.1, отличающийся тем, что в качестве раствора применяют смесь, состоящую из ионов кальция, меди и цинка, с концентрациями: 0,3-1,0 N хлорида кальция, 0,01-0,2 N хлорида меди и 0,01-0,2 N хлорида цинка.3. Способ по п.1, отличающийся тем, что в качестве раствора применяют смесь, состоящую из ионов магния, меди и цинка, с концентрациями: 0,3-1,0 N хлорида магния, 0,01-0,2 N хлорида меди и 0,01-0,2 N хлорида цинка.4. Способ по п.1, отличающийся тем, что в качестве раствора применяют смесь, состоящую из ионов кальция и меди, с концентрациями: 0,3-1,0 N хлорида кальция и 0,01-0,2 N хлорида меди.5. Способ по п.1, отличающийся тем, что в качестве раствора применяют смесь, состоящую из ионов кальция и цинка, с концентрациями: 0,3-1,0 N хлорида кальция и 0,01-0,2 N хлорида цинка.6. Способ по п.1, отличающийся тем, что в качестве раствора применяют смесь, состоящую из ионов магния и меди, с концентрациями: 0,3-1,0 N хлорида магния и 0,01-0,2 N хлорида меди.7. Способ по п.1, отличающийся тем, что в качестве раствора применяют смесь, состоящую из ионов магния и цинка, с концентрациями: 0,3-1,0 N хлорида магния и 0,01-0,2 N хлорида цинка.8. Цеолитный адсорбент, полученный способом по п.2, химического состава: Са - 1,0÷5,0%; Cu - 0,01÷0,5%; Zn - 0,01÷0,5%; Na - 5,5÷10,5%; Al - 12,0÷12,5%; Si - 13,0÷14,0%; O - 61,5÷63,0% атомных, содержащий в поверностном 1. A method of producing a zeolite adsorbent, comprising modifying type A zeolite in metal ions in a solution, drying, calcining, characterized in that the modification is carried out in solution at a mass ratio of liquid phase: solid phase, equal to 2.0-20.0, the modification process in the above solution is carried out at a temperature of 20-90 ° C, then washed, dried and calcined at a temperature of 120-550 ° C. 2. The method according to claim 1, characterized in that the mixture used is a solution consisting of calcium, copper and zinc ions, with concentrations of 0.3-1.0 N calcium chloride, 0.01-0.2 N copper chloride and 0.01-0.2 N zinc chloride. 3. The method according to claim 1, characterized in that the solution used is a mixture consisting of magnesium, copper and zinc ions, with concentrations of 0.3-1.0 N magnesium chloride, 0.01-0.2 N copper chloride and 0.01-0.2 N zinc chloride. 4. The method according to claim 1, characterized in that as a solution a mixture is used consisting of calcium and copper ions with concentrations of 0.3-1.0 N calcium chloride and 0.01-0.2 N copper chloride. The method according to claim 1, characterized in that as a solution a mixture is used consisting of calcium and zinc ions with concentrations of 0.3-1.0 N calcium chloride and 0.01-0.2 N zinc chloride. The method according to claim 1, characterized in that the mixture used is a mixture of magnesium and copper ions with concentrations of 0.3-1.0 N magnesium chloride and 0.01-0.2 N copper chloride. The method according to claim 1, characterized in that a mixture of magnesium and zinc ions with concentrations of 0.3-1.0 N magnesium chloride and 0.01-0.2 N zinc chloride is used as a solution. The zeolite adsorbent obtained by the method according to claim 2, chemical composition: Ca - 1.0 ÷ 5.0%; Cu - 0.01 ÷ 0.5%; Zn - 0.01 ÷ 0.5%; Na - 5.5 ÷ 10.5%; Al - 12.0 ÷ 12.5%; Si - 13.0 ÷ 14.0%; O - 61.5 ÷ 63.0% atomic, containing in the surface

Claims (13)

1. Способ получения цеолитного адсорбента, включающий модифицирование в растворе ионами металлов цеолита типа А, сушку, прокалку, отличающийся тем, что модифицирование осуществляют в растворе при массовом соотношении жидкая фаза:твердая фаза, равном 2,0-20,0, процесс модифицирования в вышеупомянутом растворе проводят при температуре 20-90°С, затем промывают, сушат и прокаливают при температуре 120-550°С.1. A method of producing a zeolite adsorbent, comprising modifying type A zeolite in metal ions in a solution, drying, calcining, characterized in that the modification is carried out in solution at a mass ratio of liquid phase: solid phase, equal to 2.0-20.0, the modification process in the above solution is carried out at a temperature of 20-90 ° C, then washed, dried and calcined at a temperature of 120-550 ° C. 2. Способ по п.1, отличающийся тем, что в качестве раствора применяют смесь, состоящую из ионов кальция, меди и цинка, с концентрациями: 0,3-1,0 N хлорида кальция, 0,01-0,2 N хлорида меди и 0,01-0,2 N хлорида цинка.2. The method according to claim 1, characterized in that the mixture used is a solution consisting of calcium, copper and zinc ions, with concentrations of 0.3-1.0 N calcium chloride, 0.01-0.2 N chloride copper and 0.01-0.2 N zinc chloride. 3. Способ по п.1, отличающийся тем, что в качестве раствора применяют смесь, состоящую из ионов магния, меди и цинка, с концентрациями: 0,3-1,0 N хлорида магния, 0,01-0,2 N хлорида меди и 0,01-0,2 N хлорида цинка.3. The method according to claim 1, characterized in that the mixture used is a solution consisting of magnesium, copper and zinc ions, with concentrations of 0.3-1.0 N magnesium chloride, 0.01-0.2 N chloride copper and 0.01-0.2 N zinc chloride. 4. Способ по п.1, отличающийся тем, что в качестве раствора применяют смесь, состоящую из ионов кальция и меди, с концентрациями: 0,3-1,0 N хлорида кальция и 0,01-0,2 N хлорида меди.4. The method according to claim 1, characterized in that the solution used is a mixture consisting of calcium and copper ions, with concentrations of 0.3-1.0 N calcium chloride and 0.01-0.2 N copper chloride. 5. Способ по п.1, отличающийся тем, что в качестве раствора применяют смесь, состоящую из ионов кальция и цинка, с концентрациями: 0,3-1,0 N хлорида кальция и 0,01-0,2 N хлорида цинка.5. The method according to claim 1, characterized in that the solution used is a mixture consisting of calcium and zinc ions, with concentrations of 0.3-1.0 N calcium chloride and 0.01-0.2 N zinc chloride. 6. Способ по п.1, отличающийся тем, что в качестве раствора применяют смесь, состоящую из ионов магния и меди, с концентрациями: 0,3-1,0 N хлорида магния и 0,01-0,2 N хлорида меди.6. The method according to claim 1, characterized in that the mixture used is a solution consisting of magnesium and copper ions with concentrations of 0.3-1.0 N magnesium chloride and 0.01-0.2 N copper chloride. 7. Способ по п.1, отличающийся тем, что в качестве раствора применяют смесь, состоящую из ионов магния и цинка, с концентрациями: 0,3-1,0 N хлорида магния и 0,01-0,2 N хлорида цинка.7. The method according to claim 1, characterized in that the mixture used is a mixture of magnesium and zinc ions with concentrations of 0.3-1.0 N magnesium chloride and 0.01-0.2 N zinc chloride. 8. Цеолитный адсорбент, полученный способом по п.2, химического состава: Са - 1,0÷5,0%; Cu - 0,01÷0,5%; Zn - 0,01÷0,5%; Na - 5,5÷10,5%; Al - 12,0÷12,5%; Si - 13,0÷14,0%; O - 61,5÷63,0% атомных, содержащий в поверностном слое глубиной 1-300 мкм кристаллическую фазу цеолита типа А, с катионами Са, Cu и Zn.8. The zeolite adsorbent obtained by the method according to claim 2, chemical composition: Ca - 1.0 ÷ 5.0%; Cu - 0.01 ÷ 0.5%; Zn - 0.01 ÷ 0.5%; Na - 5.5 ÷ 10.5%; Al - 12.0 ÷ 12.5%; Si - 13.0 ÷ 14.0%; O - 61.5 ÷ 63.0% atomic, containing a crystalline phase of type A zeolite in the surface layer with a depth of 1-300 μm, with Ca, Cu and Zn cations. 9. Цеолитный адсорбент, полученный способом по п.3, химического состава: Mg - 1,0÷5,0%; Cu - 0,01÷0,5%; Zn - 0,01÷0,5%; Na - 5,5÷10,5%; Al - 12,0÷12,5%; Si - 13,0÷14,0%; O - 61,5÷63,0% атомных, содержащий в поверхностном слое глубиной 1-300 мкм кристаллическую фазу цеолита типа А, с катионами Mg, Си и Zn.9. Zeolite adsorbent obtained by the method according to claim 3, chemical composition: Mg - 1.0 ÷ 5.0%; Cu - 0.01 ÷ 0.5%; Zn - 0.01 ÷ 0.5%; Na - 5.5 ÷ 10.5%; Al - 12.0 ÷ 12.5%; Si - 13.0 ÷ 14.0%; O - 61.5 ÷ 63.0% atomic, containing a crystalline phase of type A zeolite in the surface layer with a depth of 1-300 μm, with cations Mg, Cu and Zn. 10. Цеолитный адсорбент, полученный способом по п.4, химического состава: Са - 1,0÷5,0%; Cu - 0,01÷0,5%; Na - 6,0÷11,0%; Al - 12,0÷12,5%; Si - 13,0÷14,0%; O - 61,5÷63,0% атомных, содержащий в поверхностном слое глубиной 1-300 мкм кристаллическую фазу цеолита типа А, с катионами Са и Си.10. Zeolite adsorbent obtained by the method according to claim 4, chemical composition: Ca - 1.0 ÷ 5.0%; Cu - 0.01 ÷ 0.5%; Na - 6.0 ÷ 11.0%; Al - 12.0 ÷ 12.5%; Si - 13.0 ÷ 14.0%; O - 61.5 ÷ 63.0% atomic, containing a crystalline phase of type A zeolite in the surface layer with a depth of 1-300 μm, with Ca and Cu cations. 11. Цеолитный адсорбент, полученный способом по п.5, химического состава: Са - 1,0÷5,0%; Zn - 0,01÷0,5%; Na - 6,0÷11,0%; Al - 12,0÷12,5%; Si - 13,0÷14,0%; O - 61,5÷63,0% атомных, содержащий в поверхностном слое глубиной 1-300 мкм кристаллическую фазу цеолита типа А, с катионами Са и Zn.11. Zeolite adsorbent obtained by the method according to claim 5, chemical composition: Ca - 1.0 ÷ 5.0%; Zn - 0.01 ÷ 0.5%; Na - 6.0 ÷ 11.0%; Al - 12.0 ÷ 12.5%; Si - 13.0 ÷ 14.0%; O - 61.5 ÷ 63.0% atomic, containing a crystalline phase of type A zeolite in the surface layer with a depth of 1-300 μm, with Ca and Zn cations. 12. Цеолитный адсорбент, полученный способом по п.6, химического состава: Mg - 1,0÷5,0%; Cu - 0,01÷0,5%; Na - 6,0÷11,0%; Al - 12,0÷12,5%; Si - 13,0÷14,0%; O - 61,5÷63,0% атомных, содержащий в поверхностном слое глубиной 1-300 мкм кристаллическую фазу цеолита типа А, с катионами Mg и Cu.12. The zeolite adsorbent obtained by the method according to claim 6, chemical composition: Mg - 1.0 ÷ 5.0%; Cu - 0.01 ÷ 0.5%; Na - 6.0 ÷ 11.0%; Al - 12.0 ÷ 12.5%; Si - 13.0 ÷ 14.0%; O - 61.5 ÷ 63.0% atomic, containing in the surface layer with a depth of 1-300 μm a crystalline phase of type A zeolite, with Mg and Cu cations. 13. Цеолитный адсорбент, полученный способом по п.7, химического состава: Mg - 1,0÷5,0%; Zn - 0,01÷0,5%; Na - 6,0÷11,0%; Al - 12,0÷12,5%; Si - 13,0÷14,0%; O - 61,5÷63,0% атомных, содержащий в поверхностном слое глубиной 1-300 мкм кристаллическую фазу цеолита типа А, с катионами Mg и Zn. 13. Zeolite adsorbent obtained by the method according to claim 7, chemical composition: Mg - 1.0 ÷ 5.0%; Zn - 0.01 ÷ 0.5%; Na - 6.0 ÷ 11.0%; Al - 12.0 ÷ 12.5%; Si - 13.0 ÷ 14.0%; O - 61.5 ÷ 63.0% atomic, containing a crystalline phase of type A zeolite in the surface layer with a depth of 1-300 μm, with Mg and Zn cations.
RU2012144456/05A 2012-10-19 2012-10-19 METHOD FOR PRODUCING A ZEOLITE ADSORBENT AND A ZEOLITE ADSORBENT RU2012144456A (en)

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PCT/RU2013/000933 WO2014062099A1 (en) 2012-10-19 2013-10-21 Zeolite adsorbent

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CN107213866A (en) * 2017-06-26 2017-09-29 泉州师范学院 A kind of preparation method and application for being used to go the zinc oxide modified zeolite adsorbing material of anionic pollutant in water removal
CN112108124B (en) * 2020-09-26 2023-03-31 江西师范大学 Water body iron and manganese efficient adsorbent and optimization method thereof
CN117323959B (en) * 2022-06-23 2026-02-10 中国石油化工股份有限公司 A method for separating adsorbents and concentrating ethylene
CN117326569A (en) * 2022-06-23 2024-01-02 中国石油化工股份有限公司 Metal modified A-type molecular sieve and preparation method thereof

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US2882243A (en) * 1953-12-24 1959-04-14 Union Carbide Corp Molecular sieve adsorbents
US4056370A (en) * 1973-06-07 1977-11-01 Bayer Aktiengesellschaft Zeolite A with improved properties
RU2097124C1 (en) * 1993-11-02 1997-11-27 Институт катализа им.Г.К.Борескова СО РАН Method for production of sorbent and sorbent
US7014837B2 (en) * 2003-09-16 2006-03-21 E. I. Dupont De Nemours And Company Process for the production of nan-sized zeolite A
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