US2015010704A1PendingUtilityA1

Ddr zeolite seed crystal, method for producing same, and method for producing ddr zeolite membrane

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Assignee: NGK INSULATORS LTDPriority: Mar 30, 2012Filed: Sep 25, 2014Published: Jan 8, 2015
Est. expiryMar 30, 2032(~5.7 yrs left)· nominal 20-yr term from priority
C01B 37/02Y10T428/2982B01J 29/70B01D 2253/108B01D 67/0046B01D 53/228C01B 39/48B01D 2255/50B01D 67/0051B01D 69/108B01D 71/0281B01D 71/028
61
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Claims

Abstract

There are provided DDR type zeolite seed crystals capable of inhibiting generation of surplus DDR type zeolite crystals in the case of using the DDR type zeolite seed crystals as seed crystals upon forming a DDR type zeolite membrane on the surface of a porous support. The DDR type zeolite seed crystals have an average particle size of 0.05 to 1.5 μm; contain 90% or more of particles having an aspect ratio, which is obtained by dividing the maximum Feret's diameter by the minimum Feret's diameter, of 1 to 3; and have not more than 0.3 of a coefficient of variation of the square of the aspect ratio.

Claims

exact text as granted — not AI-modified
1 . A DDR type zeolite seed crystal having an average particle size of 0.05 to 1.5 μm; containing 90% or more of particles having an aspect ratio, which is a value obtained by dividing the maximum Feret's diameter by the minimum Feret's diameter, of 1 to 3; and having not more than 0.3 of a coefficient of variation of the square of the aspect ratio. 
     
     
         2 . The DDR type zeolite seed crystal according to  claim 1 , wherein the average particle size is 0.05 to 1.0 μm. 
     
     
         3 . The DDR type zeolite seed crystal according to  claim 1 , wherein a Y value calculated from the following formula (1) is not less than 60, while defining a diffraction intensity of a diffraction peak caused by (024) plane of the DDR type zeolite crystal as A, a minimum value of a diffraction intensity between the peaks of the (024) plane and (116) plane, which is influenced by an amorphous substance content, as B, and a minimum value of a diffraction intensity between the peaks of the (024) plane and (202) plane as C on the basis of the diffraction intensity obtained by X-ray diffraction analysis.
     Y =( A−C )/( B−C ).  (1)
   
     
     
         4 . A method for manufacturing a DDR type zeolite seed crystal to obtain the DDR type zeolite seed crystal according to  claim 1 , the method comprising a heating step of heating a raw material solution containing silica, and a nucleus containing a DDR type zeolite, at 130 to 180° C. for four hours or more to form the DDR type zeolite seed crystal. 
     
     
         5 . The method for manufacturing a DDR type zeolite seed crystal according to  claim 4 , wherein the nucleus is a DDR type zeolite crystal or a mixture of a DDR type zeolite crystal and amorphous silica. 
     
     
         6 . The method for manufacturing a DDR type zeolite seed crystal according to  claim 4 , wherein the raw material solution further contains 1-adamantanamine as a structure-directing agent of DDR type zeolite, and the ratio of the molar number of the 1-adamantanamine to the molar number of the silica is 0.1 or less. 
     
     
         7 . The method for manufacturing a DDR type zeolite seed crystal according to  claim 6 , wherein the DDR type zeolite seed crystal contains the 1-adamantanamine, and the specific surface area of the DDR type zeolite seed crystal containing the 1-adamantanamine is smaller than the specific surface area obtained from a particle size distribution on the assumption that the DDR type zeolite seed crystal is sphere. 
     
     
         8 . The method for manufacturing a DDR type zeolite seed crystal according to  claims 4 , further comprising a washing step of washing the formed DDR type zeolite crystal after the heating step. 
     
     
         9 . The method for manufacturing a DDR type zeolite seed crystal according to  claim 8 , wherein the washing step is a step of preparing a DDR type zeolite crystal dispersion liquid by dispersing a washed DDR type zeolite crystal in a dispersion medium to obtain a DDR type zeolite crystal-dispersed liquid having a pH of 7.5 or more. 
     
     
         10 . The method for manufacturing a DDR type zeolite seed crystal according to  claim 4 , wherein the DDR type zeolite seed crystal is manufactured without any mechanical treatment. 
     
     
         11 . A method for manufacturing a DDR type zeolite membrane, the method having an application step of applying slurry containing the DDR type zeolite seed crystal according to  claim 1  on a surface of a porous support to manufacture a seed crystal-adhered porous support. 
     
     
         12 . The method for manufacturing a DDR type zeolite membrane according to  claim 11 , wherein the average value of the opening size of pores opening on the surface of the portion of the porous support on which the seed crystal is to be applied, is not larger than the average particle size of the DDR type zeolite seed crystal. 
     
     
         13 . The method for manufacturing a DDR type zeolite membrane according to  claim 11 , comprising a DDR type zeolite membrane forming step of immersing the seed crystal-adhered porous support in a membrane-forming raw material solution containing 1-adamantanamin and silica, and heating to form a DDR type zeolite membrane, which is a DDR type zeolite membrane containing 1-adamantanamine, on the surface of the porous support. 
     
     
         14 . The method for manufacturing a DDR type zeolite membrane according to  claim 13 , wherein, in the DDR type zeolite membrane forming step, the ratio of precipitates other than the DDR type zeolite membrane to the membrane-forming raw material solution is 0.2% or less by mass. 
     
     
         15 . A method for manufacturing a DDR type zeolite seed crystal to obtain the DDR type zeolite seed crystal according to  claim 3 , the method comprising a heating step of heating a raw material solution containing silica, and a nucleus containing a DDR type zeolite, at 130 to 180° C. for four hours or more to form the DDR type zeolite seed crystal. 
     
     
         16 . A method for manufacturing a DDR type zeolite membrane, the method having an application step of applying slurry containing the DDR type zeolite seed crystal according to  claim 3  on a surface of a porous support to manufacture a seed crystal-adhered porous support.

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