# US 10,370,608 B2 · Desulfurization process using a combination of a suspension bed and a fixed bed

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- Number: US 10,370,608 B2
- Document ID: US10370608B2
- Status: Granted
- Kind: B2
- Application number: 15/861,192
- Filed: 2018-01-03
- Published: 2018-10-18
- Granted: 2019-08-06
- Earliest claimed: 2017-04-12
- Assignees: Beijing Huashi United Energy Technology and Development Co., Ltd.
- Applicants: Beijing Huashi United Energy Technology and Development Co., Ltd.
- Inventors: Ke Lin; Lin Li; Lixin Guo; Gang Zhao
- Web page: https://patentgrep.com/patent/US10370608B2

## CPC

- C10L 3/103: {Sulfur containing contaminants}
- B01D 53/52: Hydrogen sulfide
- B01D 53/75: Multi-step processes
- B01D 53/80: Semi-solid phase processes, i.e. by using slurries
- B01D 53/82: with stationary reactants
- B01D 2251/602: Oxides
- B01D 2251/604: Hydroxides
- B01D 2253/1124: Metal oxides
- B01D 2253/304: Linear dimensions, e.g. particle shape, diameter
- B01D 2255/20738: Iron
- B01D 2255/20761: Copper
- B01D 2255/20792: Zinc
- B01D 2256/24: Hydrocarbons
- B01D 2257/304: Hydrogen sulfide
- B01D 2258/05: Biogas
- C10L 2250/06: Particle, bubble or droplet size
- C10L 2290/12: Regeneration of a solvent, catalyst, adsorbent or any other component used to treat or prepare a fuel
- C10L 2290/541: Absorption of impurities during preparation or upgrading of a fuel
- C10L 2290/542: Adsorption of impurities during preparation or upgrading of a fuel
- C10L: FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G OR C10K; LIQUIFIED PETROLEUM GAS; USE OF ADDITIVES TO FUELS OR FIRES; FIRE-LIGHTERS
- B01D: SEPARATION (separating solids from solids by wet methods B03B, B03D; by pneumatic jigs or tables B03B; by other dry methods B07; magnetic or electrostatic separation of solid materials from solid materials or fluids, separation by high-voltage electric fields B03C; centrifuges, vortex apparatus B04; presses per se for squeezing-out liquid from liquid-containing material B30B9/02; treatment of water C02F, e.g. softening by ion-exchange C02F1/42; {arrangements of air intake cleaners in gas turbine plants F02C7/05} ; arrangements or mounting of filters in air-conditioning, air-humidification or ventilation F24F13/28)

## Abstract

A desulfurization process which uses both a suspension bed and a fixed bed is disclosed herein. In particular, the desulfurization slurry is mixed with a hydrogen sulfide containing gas to obtain a first mixture, and the first mixture passed into a suspension bed reactor from bottom to top, while controlling the first mixture to have a dwell time of 5-60 minutes in the reactor. A second mixture obtained by the reaction is subjected to gas liquid separation to produce a gas phase, and the gas phase is feed into a fixed bed reactor for a second desulfurization which produces purified gas. Advantageously, sulfur content in the hydrogen sulfide containing gas may be reduced from 2.4-140 g/Nm3 to 50 ppm or less by using a suspension bed, and the sulfur content may be even further reduced to less than 10 ppm in conjunction with a fixed bed.

## Claims

### Claim 1

A desulfurization process using a combination of a suspension bed and a fixed bed, comprising the following steps:
(1), mixing a desulfurizer with water uniformly to prepare a desulfurization slurry;
(2), mixing the desulfurization slurry with a hydrogen sulfide containing gas to obtain a first mixture, and passing the first mixture into a suspension bed reactor from bottom to top, with controlling the first mixture to have a dwell time of 5-60 minutes in the suspension bed reactor to allow the desulfurization slurry to contact and react sufficiently with the hydrogen sulfide containing gas;
(3), discharging a second mixture from the top of the suspension bed reactor, and subjecting the second mixture to gas liquid separation, and collecting a gas phase; and
(4), feeding the gas phase into a fixed bed reactor for carrying out a second desulfurization to obtain a purified gas.

### Claim 2 (depends on 1)

The desulfurization process of claim 1, wherein, in step (1), the desulfurizer has a particle size of no greater than 20 μm.

### Claim 3 (depends on 1)

The desulfurization process of claim 1, wherein, the desulfurizer is selected from a group consisting of amorphous iron oxide hydroxide, iron oxide, iron hydroxide or any mixture thereof.

### Claim 4 (depends on 1)

The desulfurization process of claim 1, wherein, the desulfurization slurry has a desulfurizer concentration of 1-5 wt %.

### Claim 5 (depends on 1)

The desulfurization process of claim 1, wherein, the desulfurization slurry has a desulfurizer concentration of 2-3 wt %.

### Claim 6 (depends on 1)

The desulfurization process of claim 1, wherein, the hydrogen sulfide containing gas is selected from a group consisting of biogas, coke oven gas, oilfield associated gas, natural gas, petrochemical gas or any mixture thereof.

### Claim 7 (depends on 1)

The desulfurization process of claim 1, wherein, the suspension bed reactor has an empty tower gas velocity of 0.03-0.3 m/s.

### Claim 8 (depends on 1)

The desulfurization process of claim 1, wherein, there is one suspension bed reactor, or
at least two suspension bed reactors connected in series and/or in parallel.

### Claim 9 (depends on 1)

The desulfurization process of claim 1, wherein, in step (4), the fixed bed reactor comprises a desulfurizer selected from a group consisting of amorphous iron oxide hydroxide, iron oxide, iron hydroxide, copper oxide, zinc oxide, and any mixture thereof.

### Claim 10 (depends on 1)

The desulfurization process of claim 1, wherein, the fixed bed reactor has a gas flow rate of from 1 to 20 m/s.

### Claim 11 (depends on 2)

The desulfurization process of claim 2, wherein, the desulfurizer is selected from a group consisting of amorphous iron oxide hydroxide, iron oxide, iron hydroxide or any mixture thereof.

### Claim 12 (depends on 2)

The desulfurization process of claim 2, wherein, the desulfurization slurry has a desulfurizer concentration of 1-5 wt %.

### Claim 13 (depends on 2)

The desulfurization process of claim 2, wherein, the desulfurization slurry has a desulfurizer concentration of 2-3 wt %.

### Claim 14 (depends on 2)

The desulfurization process of claim 2, wherein, the hydrogen sulfide containing gas is selected from a group consisting of biogas, coke oven gas, oilfield associated gas, natural gas, petrochemical gas or any mixture thereof.

### Claim 15 (depends on 2)

The desulfurization process of claim 2, wherein, the suspension bed reactor has an empty tower gas velocity of 0.03-0.3 m/s.

### Claim 16 (depends on 2)

The desulfurization process of claim 2, wherein, there is one suspension bed reactor, or
at least two suspension bed reactors connected in series and/or in parallel.

### Claim 17 (depends on 2)

The desulfurization process of claim 2, wherein, in step (4), the fixed bed reactor comprises a desulfurizer selected from a group consisting of amorphous iron oxide hydroxide, iron oxide, iron hydroxide, copper oxide, zinc oxide, and any mixture thereof.

### Claim 18 (depends on 2)

The desulfurization process of claim 2, wherein, the fixed bed reactor has a gas flow rate of from 1 to 20 m/s.

### Claim 19 (depends on 1)

The desulfurization process of claim 1, wherein, the suspension bed reactor has an empty tower gas velocity of 0.05-0.2 m/s.

### Claim 20 (depends on 2)

The desulfurization process of claim 2, wherein, the suspension bed reactor has an empty tower gas velocity of 0.05-0.2 m/s.
