Source: http://www.google.com/patents/US4280926?dq=7,172,682
Timestamp: 2016-12-09 02:37:00
Document Index: 357526496

Matched Legal Cases: ['arts  82', 'arts  23', 'arts  105', 'arts  62', 'arts 66', 'arts  79']

Patent US4280926 - Method for producing a catalyst and a carrier therefor - Google PatentsSearch Images Maps Play YouTube News Gmail Drive More »Sign inPatentsA method is provided for producing a catalyst and a carrier therefor in the form of sheet or honeycomb. The method comprises: beating a heat-resistant fiber such as asbesto fiber in water to form a slurry; mixing the slurry with a catalytically active agent, a carrier material therefor and/or their precursors...http://www.google.com/patents/US4280926?utm_source=gb-gplus-sharePatent US4280926 - Method for producing a catalyst and a carrier thereforAdvanced Patent SearchTry the new Google Patents, with machine-classified Google Scholar results, and Japanese and South Korean patents.Publication numberUS4280926 APublication typeGrantApplication numberUS 06/072,599Publication dateJul 28, 1981Filing dateSep 5, 1979Priority dateSep 12, 1978Also published asDE2936927A1, DE2936927C2, DE2954517C2, US4416800Publication number06072599, 072599, US 4280926 A, US 4280926A, US-A-4280926, US4280926 A, US4280926AInventorsKazunobu Abe, Tadao NakatsujiOriginal AssigneeSakai Chemical Industry Co., Ltd.Export CitationBiBTeX, EndNote, RefManPatent Citations (3), Referenced by (55), Classifications (44), Legal Events (1) External Links: USPTO, USPTO Assignment, EspacenetMethod for producing a catalyst and a carrier therefor
US 4280926 AAbstract
1. A method for producing a catalytic material for the reduction of nitrogen oxides in the presence of ammonia, which consists essentially of admixing:(a) a slurry prepared by beating at least one of inorganic heat-resistant fibers of about 1-20 mm in fiber length and of about 0.1-30 microns in diameter selected from the group consisting of asbestos fiber, silica fiber, silica-alumina fiber, chrysotile fiber, rock wool, glass fiber, anthophyllite fiber, potassium titanate fiber, carbon fiber and ceramic fiber, in water, (b) at least one powdery catalytic material having a particle size of about 0.01 to 50 microns and being an oxide selected from the group consisting of Cu, Fe, V, W and Mo or precursor thereof which is a water-insoluble, powdery compound which will be converted into catalytic material when calcined and, (c) a powdery carrier material which is at least one oxide of a metal selected from the group consisting of Ti and Al or a precursor which is a water-insoluble, powdery compound which will be converted into the oxide when calcined,thereby forming a stock material containing solid components in an amount of 1 to 10% by weight with about 80 to 40 parts by weight of fibers in relation to 20 to 60 parts by weight of the total powdery material, forming the stock into a sheet by paper-making means and drying the sheet. 2. The method as claimed in claim 1 further comprising: immersing the sheet in an impregnating slurry or solution containing catalytically active agents, carrier materials, their precursors or a mixture of at least two of these; and drying the sheet.
3. The method as claimed in claim 1 further comprising: forming the sheet into a honeycomb structure; immersing the structure in an impregnating slurry or solution containing catalytically active agents, carrier materials, their precursors or a mixture of at least two of these; and drying the structure.
4. The method as claimed in claims 2 or 3, wherein the impregnating slurry or solution further contains 1-10 parts by weight of at least one inorganic heat-resistant fiber of about 0.1-30 microns in diameter and about 0.5-5 mm in fiber length selected from the group consisting of asbestos fiber, ceramic fiber, silica fiber, silica-alumina fiber, chrysotile fiber, rock wool, glass fiber, potassium titanate fiber, anthophyllite fiber and carbon fiber, or about 0.5-5 parts of weight of polytetrafluoroethylene fiber, in relation to 100 parts by weight of the total weight of catalytically active agents, carrier materials and their precursors.
5. The method as claimed in claim 1 further comprising: forming the sheet into a honeycomb structure with an adhesive which comprises 100 parts by weight of an aqueous colloidal silica solution containing about 10-30% by weight of silica of about 1-100 millimicrons in particle size and about 10-45 millimicrons in average particle size, and 1-50 parts by weight of at least one finely divided refractory oxide particles selected from the group consisting of silica having specific surface area of 100-400 m2 /g, primary particle size of 25-150 millimicrons and average particle size of 40-200 millimicrons, alumina having specific surface area of 100-300 m2 /g, primary particle size of 10-150 millimicrons and average particle size of 30-70 millimicrons, silica-alumina having specific surface area of about 200 m2 /g, primary particle size of 1-80 millimicrons and average particle size of 10-30 millimicrons, and titania having specific surface area of about 50 m2 /g, primary particle size of 10-120 millimicrons and average particle size of 15-40 millimicrons, uniformly dispersed in the colloidal solution.
6. The method as claimed in claim 5, wherein the adhesive further contains 0.01-15 parts by weight of an organic polymer selected from the group consisting of polyethylene oxide, carboxymethylcellulose, methylcellulose and polyvinylalcohol.
Alternately, the ceramic honeycomb catalyst is produced by extruding a slurry of the catalyst forming material themselves to obviate the above disadvantage. This method provides a honeycomb catalyst having the catalytic forming material integrally incorporated therein. However, the method requires a larger amount of expensive catalyst forming material. In common with both the methods above, there is a further disadvantage in that it is difficult to handle due to its heavy weight.
It is, therefore, a general object of the present invention to obviate the disadvantages as above, and to provide an improved catalyst and a carrier therefor.
In particular, it is an important object of the present invention to provide a method for producing a catalyst in the form of sheet having the catalyst forming material uniformly dispersed therein and integrally fixed therein.
FIG. 3 is a sectional view of a further embodiment of a honeycomb structure manufactured from the sheets of FIG. 1;
As is stated hereinbefore, the stock preferably contains a binder in an amount of about 0.5-10% by weight based on the catalyst forming material in the stock. The binders suitably used in the invention are inorganic binders such as alumina sol, silica sol and titania sol, and organic binders, in particular, synthetic rubbers such as acrylonitrile-butadiene rubber (NBR) and styrene-butadiene rubber (SBR). The stock may further contain a fixing agent and/or a sizing agent. The fixing agent preferably used in the invention are organic cationic polyelectrolytes such as polyacrylamine, polyamine, polyamine- and polyamide-epichlorohydrin condensation polymer and polyethyleneimine. The polyamine includes condensates of alkylene dichlorides with alkylenepolyamines such as ethylenediamine, tetramethylenediamine and hexamethylenediamine, poly(N,N-dimethyl- and diethylaminomethacrylate), polyvinylimidazolein, polyvinylpyridine, cycloaddition polymers of diallylamine, copolymers of N-vinylpyrolidone and acrylamide, and their quaternary salts such as halides and ammoniums. Inorganic fixing agents such as aluminum sulfate and ferric sulfate are also preferably used in the invention. The amount of the fixing agents in the stock is preferably in the range of about 2-10% by weight based on the catalyst forming material therein. The stock may contain a sizing agent in an amount of 0.01-1% by weight based on the solid components, i.e., the fiber and the catalyst forming material in the stock. Rosins and organosilicone polymer, for example, polysiloxanes, are used as the sizing agent. The fixing agent and the sizing agent are added usually in the form of aqueous emulsion or solution to the slurry of the fiber and the catalyst forming material.
The stock thus obtained is formed into a dried sheet by a conventional paper making machine as usual such as the cylinder machine, the Fourdrinier machine and the short wire machine. The stock may be hand-made into a sheet by a hand mound, when needed. The sheet is dried usually at temperatures of about 60-150° C. When a fiber of a high melting point is used, however, the sheet may be dried at higher temperatures.
According to the invention, the sheet thus obtained may be further coated or impregnated with the catalyst forming material so as to support the material on or in the sheet in a larger amount before or after the sheet is formed into a honeycomb structure. More particularly, the sheet or the honeycomb manufactured therefrom is immersed in a slurry or a solution containing about 50-500 g/l of the catalyst forming material, the excess amount of the slurry or solution removed from the substrate, dried, and if necessary, calcined to convert the precursor into the active form. When desired, the above process is repeated. The sheet, after coating or immersing, is dried preferably with air passed thereon or therethrough so that the material coated or impregnated has a uniform distribution over the sheet. The electromagnetic drying is also preferably employed. The drying temperature is usually about 80-200° C., but may be higher than the temperature, depending on the fiber and the additives.
According to the present invention, an improved adhesive is used on manufacturing a honeycomb structure from the sheet of the invention. The adhesive of the invention comprises 100 parts by weight of an aqueous colloidal solution containing about 10-30% by weight, preferably about 20-30% by weight, of silica based on the solution having about 1-50 parts by weight, preferably about 2-20 parts by weight, of at least one finely divided refractory oxide selected from the group consisting of silica, alumina, silica-alumina and titania uniformly dispersed therein. The colloidal silica solution, as is well known, contains fine silica particles of about 1-100 millimicrons in particle size and about 10-45 millimicrons in average particle size dispersed in water. A marketed example of the solution is, for example, Snowtex No. 30 (Nissan Kagaku) which contains about 30% by weight of silica, and is preferably used in the invention.
Finely divided silica, also known as white carbon, used in the invention preferably has a very large specific surface area of about 100-400 m2 /g, a primary particle size of about 25-150 millimicrons and an average particle size of about 40-200 millimicrons. Marketed products such as Syloid (Shiraishi Kogyo), Aerosil 2000 (Japan Aerosil) can be used. Finely divided alumina used in the invention preferably has a specific surface area of about 100-300 m2 /g, a little smaller than that of a γ-alumina, a primary particle size of about 10-150 milimicrons and an average particle size of about 30-70 millimicrons. A marketed product, Alumina Oxide C (Japan Aerosil), is one of the suitably used alumina in the invention. Finely divided silica-alumina used in the invention has a specific surface area of about 200 m2 /g, a little smaller than that of the finely divided silica, a primary particle size of about 1-80 millimicrons and an average particle size of about 10-30 millimicrons. Marketed products such as Aerosil COK 84 and Aerosil MOX 170 (both Japan Aerosil) can be used in the invention. Finely divided titania used in the invention has preferably a specific surface area of about 50 m2 /g, a primary particle size of about 10-120 millimicrons and an average particle size of about 15-40 millimicrons. A marketed product such as Titanium P25 (Japan Aerosil) can be used.
The adhesive preferably further contains about 0.01-15 parts by weight, more preferably, about 0.05-5 parts by weight, of an water-soluble organic polymer relative to 100 parts by weight of the colloidal silica solution so as to increase the adhesive force thereof. The polymer also serves to increase the viscosity of the adhesive, thereby permitting the control of the permeation of the adhesive into the sheet and improving the productivity in manufacturing a honeycomb structure. The water-soluble polymers used in the invention are preferably polyethylene oxide of molecular weight of about 10000--100000, carboxymethylcellulose of polymerization degree of about 300-500, methylcellulose of polymerization degree of about 70-650, and polyvinylalcohol of polymerization degree of about 100-200. The adhesive of the invention preferably has a viscosity of about 10-500 cp., and is usually applied in an amount of 10-400 g/m2.
As has been described above, according to the invention, a higher catalytic activity is provided with the heat-resistant sheet such as asbestos sheet. This is a remarkable contrast with the sheet catalyst in which the catalyst forming material is carried in the sheet after the sheet forming. Furthermore, according to the invention, the catalyst forming material is coated on the sheet or the honeycomb in a thickness of about 50-100 microns, much smaller than the prior art, to provide a higher catalytic activity. This is also a remarkable contrast with the prior catalyst which has a thick coating thereon of the catalyst forming material, but a low activity.
Fifty grams of asbestos fiber of about 8 microns in diameter and about 2 mm in average length were sufficiently beaten in 2 l of water, and to the resultant slurry was added 50 g of anatase titania powder of 0.5 microns in average particle size, and 7 g of vanadium pentoxide of about 3 microns in average particle size, and thoroughly mixed therewith. The slurry was further mixed with ammonia water to adjust pH thereof to about 8, and was added thereto 0.7 g of Lufax 295, a cationic polyelectrolyte sold by Rohm & Haas Co., and then sulfuric acid to further adjust pH of the mixture to about 4, followed by the addition of 1 g of Nipol 1571, an acrylonitrile-butadiene copolymer binder sold by Nihon Geon, thus fixing the oxides in the fiber. The thus obtained stock slurry was hand-made into a sheet by a hand mould, and dried.
The thus obtained sheet of 0.3 mm in thickness and 260 g/m2 was then corrugated and formed into a single-faced corrugated board, as is shown in FIG. 1, by a conventional corrugating machine using silica sol as a binder. The corrugated board was then formed into a honey-comb structure manually by use of the silica sol, thereby providing a honeycomb catalyst A having a volume of 86 ml and an equivalent honeycomb diameter of 4 mm.
Another slurry for immersing therein the carrier was prepared by mixing 5 g of vanadium pentoxide with 45 g of anatase titania in 250 ml of water in a stainless beaker, and stirring the mixture for 1 hr with the aid of 50 ml of glass beads added thereto. The honeycomb carrier was then immersed in the slurry, the excess thereof removed from the honeycomb, and dried. The honeycomb was immersed again in the slurry and dried, thus providing a honeycomb catalyst B having 4.2 g of the oxides therein.
The same asbestos fibers (1.5 Kg) as used in EXAMPLE 1 was sufficiently beaten in 30 l of water, and to the resultant slurry were added and mixed therewith 500 g of anatase titania of the same size as used in EXAMPLE 1, 21 g of Lufax 295, and then sulfuric acid to arrange pH of the mixture to about 5, and then 10 g of Nipol 1571. The thus obtained stock was hand-made into a sheet of 1 mm in thickness and 660 g/m2.
The sheets obtained were fixed parallel to each other in a basket of capacity of 84 ml so as to form a honeycomb structure as is shown in FIG. 4. The honeycomb structure was then immersed in the same slurry as used in EXAMPLE 2 and dried in the same manner as in EXAMPLE 2, thus providing a honeycomb catalyst C having 4.8 g of the oxides carried therein.
Thirty grams of alumina powder of about 0.1 microns in average particle size (Caeser), 67 g of asbestos fiber, the same as used in EXAMPLE 1, 3.5 g of Nipol 1571 and 1.5 g of alumina sol were thoroughly mixed in 2.5 l of water while sufficiently beating the fiber. The thus obtained stock was then hand-made into a sheet of 0.3 mm in thickness and 270 g/m2.
In this example an improved adhesive was used to manufacture a honeycomb structure from the above sheet. The adhesive used as prepared by adding 5 g of Aerosil 2000, finely divided silica sold by Japan Aerosil, to 100 g of Snowtex No. 30, an aqueous colloidal silica solution containing about 30% by weight of silica sold by Nissan Kagaku, and mixed thoroughly by the use of a micro-agitor for 10 min.
Ten grams of tungsten trioxide, 40 g of γ-alumina, 4 g of glass fiber of 0.3 mm in average length and of about 6 microns in diameter, and 200 ml of water were thoroughly mixed in a stainless beaker for 20 min. together with 50 ml of glass beads. In the thus prepared slurry was immersed the same honeycomb carrier as obtained in EXAMPLE 2, the excess amount of the slurry removed from the honeycomb, dried at a temperature of 40° C. for 3 hrs. while forcing air to pass through the honeycomb at a linear velocity of about 3 m/sec, thus providing a honeycomb catalyst E having 8.5 g of the oxides carried therein.
A marketed astestos sheet of 0.3 mm in thickness and 150 g/m2 in basis weight (Japan Asbestos) was formed into a honeycomb structure of the same size in the same manner as in EXAMPLE 1. The honeycomb was the immersed in the same slurry containing titania and vanadium pentoxide as used in EXAMPLE 2, the excess amount of the slurry removed from the honeycomb, and dried. After the repetition of the immersion four times, a honeycomb catalyst R was obtained which had 4.1 g of the catalyst forming material.
The catalytic activity of the catalysts obtained above in terms of the conversion of nitrogen monoxide into nitrogen and water in the presence of ammonia as a reducing agent was estimated. Each of the catalysts for the estimation was charged in a Pyrex tube of 50 mm in inner diameter with a heat insulator wrapped therearound to maintain the temperature therein constant. A gas mixture consisting of 200 ppm of nitrogen monoxide, 200 ppm of ammonia, 10% by volume of water vapor, 12% by volume of carbon dioxide, 1000 ppm of sulfur dioxide, and the residue nitrogen was passed through the catalyst at a temperature of 350° C. at a space velocity of 10000 hr.-1 (converted value at room temperature). The conversion of nitrogen monoxide (NO conversion) was calculated from the following equation: [(NO concentration at the inlet)-(NO concentration at the outlet)]/(NO concentration at the inlet)×100 (%). The results are shown in TABLE 1.
The coated surfaces of the above catalysts were scratched by pencils of hardness 2H and HB, respectively, under the load of 100 g, to observe whether scratches appeared. The results are shown in TABLE 2.
TABLE 2______________________________________    2H           HB______________________________________B          appeared       not appearedC          "              "E          not appeared   "F          "              "R          appeared       appeared______________________________________
For the purpose of comparison, the adhesive strengths were estimated in the same manner as in above on the adhesive (p) having an insufficient amount of the refractory oxide; (q) consisting of Snowtex No. 30 only; (r) consisting of Alumina Sol No. 20 containing about 20% by weight of alumina (Nissan Kagaku); and (s) consisting of 100 parts by weight of Alumina Sol No. 20 and 5 parts by weight of Aluminum Oxide C.
TABLE 3______________________________________                         Adhesive                         strengthsRefractory oxides* PEO 8      (g)______________________________________a     5 parts silica              58b     5 parts alumina             19c     5 parts silica-alumina      64d     5 parts titania             45e     5 parts silica   0.5 parts  82f     5 parts alumina  0.5 parts  23g     5 parts silica-alumina                  0.5 parts  105h     5 parts titania  0.5 parts  62i     1 part silica-alumina       21j     10 parts silica-alumina     68k     50 parts silica-alumina     401     5 parts titania  0.01 parts 66m     5 parts titania  0.1 parts  79n     5 parts titania  5 parts    **o     5 parts titania  10 parts   **p     0.5 parts silica-alumina    9q                                 7r                                 &lt;1s                                 1______________________________________ *Aerosil 2000, Aluminum Oxide C, Aerosil COK 84 and Titanium Oxide P25 were used as finely divided refractory oxides, silica, alumina, silicaalumina and titania, respectively. **The adhesive strength was too large to cause the tearing of the sheets.
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B01J35/04Legal EventsDateCodeEventDescriptionMar 19, 1981ASAssignmentOwner name: SAKAI CHEMICAL INDUSTRY CO., LTD., 1, EBISUJIMA-CHFree format text: ASSIGNMENT OF ASSIGNORS INTEREST.;ASSIGNORS:ABE KAZUNOBU;NAKATSUJI TADAO;REEL/FRAME:003841/0148Effective date: 19810109RotateOriginal ImageGoogle Home - Sitemap - USPTO Bulk Downloads - Privacy Policy - Terms of Service - About Google Patents - Send FeedbackData provided by IFI CLAIMS Patent Services