# US 7,608,236 B2 · Method for producing hydroxylammonium salts

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- Number: US 7,608,236 B2
- Document ID: US7608236B2
- Status: Granted
- Kind: B2
- Application number: 10/562,984
- Filed: 2004-07-28
- Published: 2007-07-26
- Granted: 2009-10-27
- Earliest claimed: 2003-08-01
- Assignees: Domo Caproleuna GmbH
- Inventors: Wolfgang Löbel; Thomas Strecker; Joachim Seidler
- Web page: https://patentgrep.com/patent/US7608236B2

## CPC

- B01J 8/222: {in the presence of a rotating device only}
- B01F 23/233: using driven stirrers with completely immersed stirring elements
- B01F 35/93: arranged inside the receptacle
- C01B 21/1418: {by catalytic reduction of nitrogen oxides or nitrates with hydrogen}
- B01F 23/23362: {the gas being introduced under the stirrer}
- B01F 27/1123: sickle-shaped, i.e. curved in at least one direction
- B01F 27/118: Stirrers in the form of brushes, sieves, grids, chains or springs
- B01F 27/192: with dissimilar elements
- B01F 2215/0422: Numerical values of angles
- B01F 2215/0431: Numerical size values, e.g. diameter of a hole or conduit, area, volume, length, width, or ratios thereof
- B01J 21/18: Carbon
- B01J 23/42: Platinum
- B01J 2208/00141: Coils
- B01J 2208/0084: inside the bed, e.g. baffles
- B01J 2208/00867: inside the bed, e.g. rotary mixer
- B01J 2219/0025: Foam formation
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01F: MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING (mixing paints B44D3/06)
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}

## Abstract

A method of producing hydroxylammonium salts by catalytic reaction of nitrogen monoxide with hydrogen in a diluted aqueous solution of mineral acid in the presence of platinum catalysts suspended on a support in multiple subsequent reaction stages. This reaction takes place in a stirred reactor wherein a gas inlet and distribution system is provided in the lower part of the stirred reactor, a disk agitator is placed immediately above, the hub with bearing surface or support mounting angled, concave and tilted agitator blades that rotate their angled or concave sides in the direction of motion, and a two-blade agitator is provided on the agitator shaft in the upper part of the stirred reactor, its individual leaves being offset like lamellas so that they constantly wet the reactor cap when rotating.

## Claims

### Claim 1

A method for producing hydroxylammonium salts by reacting nitrogen monoxide (NO) with a molar hydrogen surplus in a reaction vessel in an aqueous medium of strong mineral acids in the presence of a noble metal catalyst suspended on a carbon-based support at excess pressure up to 10 bar and temperatures up to 80° C., the hydroxylammonium salt being constantly removed from the reaction vessel, said reaction vessel being a stirred reactor with an agitator shaft and agitator blades attached to the agitator shaft via a hub and bearing surface or support, characterized in that:
a gas inlet and distribution system is provided in a lower part of the stirred reactor,
a disk agitator is placed immediately above the gas inlet and distribution system,
the disk agitator comprising the hub, said hub comprising the bearing surface or support with angled, concave and tilted agitator blades that rotate angled and concave sides in a direction of motion, and
a two-blade blade agitator is provided on the agitator shaft in an upper part of the stirred reactor, individual leaves of the blade agitator being offset like lamellas at an angle of 0 to 30° C. to a blade axis so that they constantly wet a reactor cap when rotating.

### Claim 2 (depends on 1)

The method according to claim 1 wherein sulfuric acid at a 4 to 5-normal concentration is used as the strong mineral acid and the product is hydroxylammonium sulfate.

### Claim 3 (depends on 1)

The method for producing hydroxylammonium salts according to claim 1 wherein hydrogen and NO are used at a molar ratio of 1.9 to 2.0: 1.0.

### Claim 4 (depends on 1)

The method for producing hydroxylammonium salts according to claim 1 wherein the suspended catalyst (including its support) is used in a liquid suspension at 7 to 50 g/l and a mean diameter of 30 to 80 pm.

### Claim 5 (depends on 1)

The method for producing hydroxylammonium salts according to claim 1 wherein platinum is used as a noble metal catalyst at a concentration of 0.1 to 0.5 percent by weight in relation to its carbon support.

### Claim 6 (depends on 1)

The method for producing hydroxylammonium salts according to claim 1 wherein gases escape from an annular gas inlet and distribution system with an average gas bubble diameter of 5 mm to 6 mm and a gas speed of 7 to 30 m/sec.

### Claim 7 (depends on 1)

The method for producing hydroxylammonium salts according to claim 1 wherein 6 concave and tilted agitator blades are attached to the rotating hub of the disk agitator.

### Claim 8 (depends on 1)

The method for producing hydroxylammonium salts according to claim 1 wherein wall baffles are arranged in the stirred reactor.

### Claim 9 (depends on 1)

The method for producing according to claim 1 wherein the two-blade blade agitator in the top portion of the stirred reactor is placed at an angle of incidence of 45° to 90° in relation to a liquid level in the reactor, wherein the blade agitator consists of offset individual lamella-like leaves, and wherein the blade agitator diameter is 0.3 to 0.4 relative to the reactor diameter.

### Claim 10 (depends on 1)

The method for producing hydroxylammonium salts according to claim 1 wherein a blade height of the individual leaves of the blade agitator is 0.2 to 0.5 relative to a diameter of the blade agitator.

### Claim 11 (depends on 1)

The method for producing hydroxylammonium salts according to claim 1 wherein the disk agitator in the bottom portion of the reactor is operated at a peripheral speed of 5 to 15 m/sec.