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United States Patent (19) 11 Patent Number: 5,278,112 Klatte (45) Date of Patent: Jan

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United States Patent (19) 11 Patent Number: 5,278,112 Klatte (45) Date of Patent: Jan III US0052781 12A United States Patent (19) 11 Patent Number: 5,278,112 Klatte (45) Date of Patent: Jan. 11, 1994 (54 CHEMICALLY IMPREGNATEDZEOLITE Primary Examiner-Carl F. Dees AND METHOD FOR CHEMICALLY Attorney, Agent, or Firm-Limbach & Limbach IMPREGNATING AND COATING ZEOLITE 57) ABSTRACT 76) Inventor: Fred Klatte, Two Spruce St., San A process for impregnating zeolite with permanganate, Francisco, Calif. 941 18 such as potassium permanganate, and a product of such process. The process preferably includes the steps of (21) Appl. No.: 975,680 dehydrating zeolite crystals to have about 5% moisture 22 Filed: Nov. 13, 1992 content, mixing the dehydrated zeolite crystals with solid permanganate (preferably potassium permanga 51) Int. Cl.......................... B01J 29/04; B01J 37/02 nate crystals), immersing the solid mixture in, or spray 52 U.S. Cl. ......................................... 502/62; 502/60 ing the solid mixture with, water at about 190 F. and 58) Field of Search .............................. 502/60, 62, 86 mixing the resulting slurry, and then drying the mixed 56) References Cited slurry to produce permanganate-impregnated Zeolite crystals having about 15% moisture content. In other U.S. PATENT DOCUMENTS preferred embodiments, the inventive method includes 3,049,399 8/1962 Gamson et al. ......................... 21/53 the steps of impregnating zeolite with a quaternary ammonium cation (QAC) and then coating the impreg FOREIGN PATENT DOCUMENTS nated zeolite with permanganate, or impregnating zeo 0063436 10/1982 European Pat. Off............... 502/60 lite with permanganate and then coating the impreg 0188138 7/1986 European Pat. Off. .... 502/60 nated zeolite with a QAC. Either coating acts as a pro 0067521 6/1981 Japan ................... ... SO2/60 tective agent for the impregnating substance in each 0000827 1/1985 Japan ..................................... 502/60 zeolite crystal's interior, and allows regulated time re OTHER PUBLICATIONS lease control of the impregnating substance, thus per mitting a controlled diffusion (or absorption) rate in Material Safety Data Sheet (5 pages), Chemax, Inc. applications in which the coated, impregnated zeolite is (Jan. 30, 1992). employed to absorb contaminants from air or water. Cadena, et al., Treatment of Waters Contaminated with Combinations of coated and uncoated zeolite crystals BTX and Heavy Metals Using Tailored Zeolites, Feb. can be chosen to match specific environmental circum 1992, New Mexico Waste-Management Education and stances calculable by analysis of the air or water to be Research Consortium, Technical Completion Report treated. Mixtures of coated and uncoated QAC-impreg (Project No. WERC-91–41), 22 pages. nated zeolite can be used to react with organics such as Gao, et al., Use of Tailored Zeolites for Removal of Ben benzene, toluene, and xylene, and mixtures of coated zene and Toluene from Water, 45th Purdue Industrial and uncoated permanganate-impregnated zeolite can be Waste Conference Proceedings, pp. 509-515, Lewis used to react with hydrogen sulfide, acetone, ethylene Publishers, Inc. Chelsea, Mich., 1991. glycols, formaldehyde, and other contaminants. Brochure entitled "Carusorb (R) 200," by Carus (1 page). 38 Claims, 1 Drawing Sheet 5,278,112 1. 2 tassium permanganate. However, we have recognized CHEMICALLY IMPREGNATED ZEOLTE AND that, under certain conditions, such permanganate METHOD FOR CHEMICALLY MPREGNATING impregnated zeolite reacts too rapidly to be practically AND COATING ZEOLITE useful for some air filtration applications. For example, when air contaminated with 50 ppm of hydrogen sulfide FIELD OF THE INVENTION is caused to flow (at a rate of 15 liters per minute) The invention relates to processes for producing through a bed of the inventive permanganate-impreg chemically impregnated zeolite and coated, chemically nated zeolite crystals (where the crystals have size impregnated zeolite, and to the products of such pro about 0.25 inch X 0.125 inch, and the bed has volume of cesses. A preferred embodiment of the invention is a O 75 cubic centimeters, and dimensions 1'(1d)x6"), the process for chemically impregnating zeolite crystals crystals typically become saturated with hydrogen sul with either a quaternary ammonium cation or a perman fide within about 48 hours. Although the impregnated ganate, and then coating the impregnated zeolite crys zeolite crystals usefully absorb hydrogen sulfide from tals with the other of these two substances. air, the hydrogen sulfide absorption rate is significantly 15 higher than can be achieved using conventional per BACKGROUND OF THE INVENTION manganate-impregnated alumina products, and is unde Zeolites are hydrated metal aluminosilicate con sirably high for some applications. pounds with well-defined (tetrahedral) crystalline struc For both air (and other gas) and water filtration appli tures. Because Zeolite crystals (both natural and syn cations, it would be desirable to reduce the rate at thetic) have a porous structure with connected channels -which permanganate-impregnated zeolite absorbs se extending through them, they have been employed as lected contaminants, and to control such absorption molecular sieves for selectively absorbing molecules on rate. Similarly, it would be desirable to reduce the rate the basis of size, shape, and polarity. at which QAC-impregnated zeolite absorbs selected Volumes packed with zeolite crystals (for example, contaminants, and to control such absorption rate. small zeolite crystals chosen to have size in the range 25 However, until the present invention, it was not known from 0.2 mm to several millimeters) have been en ployed in water and air (or other gas) filtration systems how to achieve either of these objectives. to selectively absorb contaminants from a flowing SUMMARY OF THE INVENTION stream of water or gas. It has been proposed to treat zeolite crystals by im In one class of embodiments, the invention is a pro pregnating them with quaternary ammonium cations cess for impregnating zeolite crystals with a permanga (such as tetramethylammonium, tetraethylammonium, nate, such as potassium permanganate. The product of hexadecyltrimethylammonium, dibenzyldimethylam such process is another embodiment of the invention. A nonium, benzyltriethylammonium, and cetyltrime preferred embodiment of the inventive process results thylammonium), to enhance the zeolite's capacity to 35 in zeolite crystals uniformly impregnated with potas absorb heavy metal, benzene, toluene, and xylene con sium permanganate (having a potassium permanganate taminants from water. See, for example, Cadena, et al., content of about 4% and a moisture content of about "Treatment of Waters Contaminated with BTX and 15%), and includes the following steps: dehydrating the Heavy Metals Using Tailored Zeolites,' New Mexico zeolite crystals until they have about 5% moisture con Waste-management Education and Research Consor tent, then mixing the dehydrated zeolite crystals with tium Technical Completion Report for Project No. solid potassium permanganate (preferably with a weight WERC-91-41 (February 1992). If not impregnated with ratio P/T substantially equal to 4%, where P is the a quaternary ammonium cation (QAC), zeolite does not potassium permanganate weight and T is the total function adequately as a molecular sieve for organic weight of the final product of the process), immersing chemicals such as benzene, toluene, and xylene. 45 the solid zeolite and permanganate mixture in (or spray It has also been proposed to impregnate an aqueous ing the solid mixture with) water whose temperature is solution of permanganate (such as permanganate of above room temperature (preferably the water tempera potassium, sodium, magnesium, calcium, barium, or ture is about 190 F), thoroughly mixing the resulting lithium) into pores of substrates such as silica gel, alu slurry, and finally air drying the mixed slurry to pro mina, silica-alumina, activated bauxite, and activated 50 duce permanganate-impregnated zeolite crystals having clay. The resulting impregnated porous substrates have about 15% moisture content. Typically, four pounds of been employed for filtering and deodorizing air. See, for potassium permanganate, fifteen pounds of water, and example, U.S. Pat. No. 3,049,399, issued Aug. 14, 1962, 86 pounds of dehydrated (5% moisture) zeolite crystals to Gamson, et al. are employed to produce each 100 pounds of the prod However, zeolite crystals have not been impregnated 55 uct of this process. (throughout their volume) with permanganate. Variations on the preferred embodiment described Further, because permanganates are strong oxidizing above produce zeolite crystals uniformly impregnated agents, those skilled in the art have avoided exposing with potassium permanganate, having a potassium per quaternary ammonium cations or salts to permanga manganate content greater than 4%, and preferably, as nates (to avoid violent reactions of the type predicted in high as in the range from 8% to 10%. In these varia the literature). For this reason, it has not been proposed tions, the dehydrated zeolite crystals are mixed with to treat a permanganate-impregnated substrate (such as solid potassium permanganate with a weight ratio P/T permanganate-impregnated zeolite) with a quaternary greater than 4%, where P is the potassium permanga ammonium cation or salt. Nor has it been proposed to nate weight and T is the total weight of the final prod treat a substrate impregnated with a QAC (quaternary 65 uct of the process.
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