CN105233649A - Chelated iron desulfurizer and application method thereof - Google Patents
Chelated iron desulfurizer and application method thereof Download PDFInfo
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- CN105233649A CN105233649A CN201510633365.2A CN201510633365A CN105233649A CN 105233649 A CN105233649 A CN 105233649A CN 201510633365 A CN201510633365 A CN 201510633365A CN 105233649 A CN105233649 A CN 105233649A
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Abstract
The invention discloses a chelated iron desulfurizer and application method thereof, and belongs to the technical field of gas purification. The chelated iron desulfurizer comprises the following components: soluble iron salt, an iron salt chelating agent, a sulfide absorbent, a stabilizing agent, a composite particle settling agent, and a multifunctional corrosion inhibitor; wherein the mole ratio of Fe<3+> to Fe<2+> in soluble iron salts is 1:3-5:1; the mole ratio of chelating agent to iron salts is 1.2:1-3:1, and the pH value of the solution is 8.0 to 9.5. The chelated iron desulfurizer is used to remove sulfur under the assistance of a hyper-gravity technology; the desulfurization efficiency is high, the work sulfur capacity is high, the performance of the desulfurizer is stable, and the oxidation regeneration performance is good. The hyper-gravity chelated iron desulfurization technology has the advantages that the technology is simple, the mass transfer efficiency between gas and liquid is high, the equipment is small and can be easily assembled or disassembled, and the technology can be used to remove H2S from natural gas or associated gas in an offshore oil and gas platform.
Description
Technical field
The present invention relates to a kind of Complexing Iron desulfurizing agent and using method thereof, belong to gas purification technique field.
Background technology
The research in Complexing Iron desulfurizing agent is had in prior art:
The iron chelating agent that the LO-CAT technique doctor solution of Wheelabrator cleaning air system company of U.S. exploitation adopts is ethylenediamine tetra-acetic acid and N-hydroxyethyl-ethylenediamine triacetic acid, and have good sequestering power to iron, desulfuration efficiency is very high; But desulfurization operations cost is higher, and Sulfur capacity is lower.
The SulFerox technique of ShellOil and DowChemical company exploitation, and the iron chelating agent that the iron chelating agent doctor solution of the Sulfint technique doctor solution employing of Technical University of Vienna and the cooperative development of Austrian Consolidated Engineering Company, Inc. adopts is all EDTA, be characterized in that palliating degradation degree is little, chelating capacity is large, add the concentration of Complexing Iron in doctor solution, decrease liquid circulation amount.
In the DDS sulfur removal technology doctor solution of Chemical and Molecular Engineering College of Beijing Univ.'s exploitation, iron chelating agent adopts porphyrin, ferroheme etc., and the method desulfuration efficiency is high, environment friendly and pollution-free; But doctor solution less stable.
Summary of the invention
The present invention aims to provide a kind of Complexing Iron desulfurizing agent, present invention also offers the using method of this desulfurizing agent, removes hydrogen sulfide gas under being suitable for super gravity field.
The invention provides a kind of Complexing Iron desulfurizing agent, it is made up of following component: soluble ferric iron salt, molysite chelating agent, sulphur compound absorbent, stabilizing agent, compound sulfur granules sedimentation agent and multi-functional corrosion inhibior; Fe is contained in soluble ferric iron salt in desulfurizing agent
3+with Fe
2+; The mol ratio of chelating agent and molysite is 1.2:1 ~ 3:1; Each component proportion is as follows:
Soluble ferric iron salt: 2.2 ~ 12 parts,
Molysite chelating agent: 5 ~ 20 parts;
Sulphur compound absorbent: 15 ~ 70 parts;
Stabilizing agent: 0.1 ~ 15 part;
Compound sulfur granules sedimentation agent: 0.05 ~ 2 part;
Multi-functional corrosion inhibior: 0.05 ~ 5 part.
Further, Fe in described soluble ferric iron salt
3+with Fe
2+mol ratio be 1:3 ~ 5:1, wherein provide Fe
3+be FeNH
4(SO
4)
212H
2o or Fe
2(SO
4)
3in at least one, wherein provide Fe
2+be Fe (NH
4)
2(SO
4)
26H
2o.
Further, described chelating agent is EDTA, Na
4eDTA, NTA, Na
3nTA, HEDTA, Na
3one or more in HEDTA, DTPA, HEDP, TEA, citric acid, natrium citricum, sulfosalicylic acid, sulfosalicylic acid sodium salt, gluconic acid.
Further, described sulphur compound absorbent is NaOH, Na
2cO
3, NaHCO
3, KOH, K
2cO
3, KHCO
3in one or more.
Further, described stabilizing agent is one or more in imidazoles, benzoate, alkali metal chlorizated salt, alkali metal thiosulfate.
Further, described compound sulfur granules sedimentation agent is made up of the initator that flocculates, flocculation flocculating agent, flocculating setting agent:
Described flocculation initator is one or both in sublimed sulfur, shitosan, and content is 12% ~ 20% of sulfur granules sedimentation agent;
Described flocculation flocculating agent is AlCl
3, one or both in sodium metasilicate, content is 3% ~ 32% of sulfur granules sedimentation agent;
Described flocculating setting agent is two or more in PAM, straight chain decyl alcohol, polyglycol ether, straight chain hexadecanol, and content is 55% ~ 84% of sulfur granules sedimentation agent.
Further, described multi-functional corrosion inhibior helps corrosion inhibiter, antibacterial type corrosion inhibiter, stable potential corrosion inhibiter to form by the main corrosion inhibiter of stable complexation iron, stable complexation iron:
Described main corrosion inhibiter is one or more the mixture in alkali metal sulfates, tungstates, and content is 27% ~ 57% of multi-functional corrosion inhibior;
The described corrosion inhibiter that helps is one or more mixture in alkali metal benzoate, silicate, and content is 3% ~ 15% of multi-functional corrosion inhibior;
Described antibacterial type corrosion inhibiter is one or more the mixture in KBr, KI, formaldehyde, and content is 18% ~ 66% of multi-functional corrosion inhibior;
Described stable potential corrosion inhibiter is one or both in dodecyl sodium sulfate, paratoluenesulfonic acid sodium salt, and content is 3% ~ 11% of multi-functional corrosion inhibior.
The invention provides a kind of using method of Complexing Iron desulfurizing agent, comprise the following steps:
(1) the Complexing Iron desulfurizing agent in fluid reservoir is pumped into desulfurization cross_flow rotating packed bed and gas flow for 2Nm with the flow of 20 ~ 80L/h
3/ h H 2 S-containing gas is counter current contacting in the filler of rotary drum, and the alkaline solution absorption that hydrogen sulfide gas is desulfurized in agent is converted into HS
-, be desulfurized the Fe in agent
3+l is oxidized to sulphur simple substance, the Fe in desulfurizing agent
3+l is reduced to Fe
2+l;
(2) remove the gas after hydrogen sulfide emptying after the built-in demister of cross_flow rotating packed bed, Complexing Iron sulfur removing pregnant solution pumps into regeneration cross_flow rotating packed bed and air counter current contacting in the filler of rotary drum with the flow of 20 ~ 80L/h, the Fe in desulfurizing agent
2+l is oxidized to Fe again by the oxygen in air
3+l, regeneration temperature is 40 ~ 50 DEG C;
(3) desulfurizing agent after regeneration is pumped in fluid reservoir, add compound sulfur granules sedimentation agent, make sulphur rapid flocculation be deposited to bottom reservoir, then pump in filter, the sulphur cake formed carries out subsequent treatment, and filtrate returns fluid reservoir and carries out next circulation desulfurization process.
Further, total concentration of iron 2.2 ~ 12g/L of soluble ferric iron salt, wherein Fe in described Complexing Iron desulfurizing agent
3+with Fe
2+mol ratio be 1:3 ~ 5:1; Chelating agent concentrations 5 ~ 20g/L; Sulphur compound absorbent concentration 15 ~ 70g/L; Stabilizer concentration 0.1 ~ 15g/L; Compound sulfur granules sedimentation agent concentration 0.05 ~ 2g/L; Multi-functional corrosion inhibior concentration 0.05 ~ 5g/L; The mol ratio of chelating agent and molysite is 1.2:1 ~ 3:1; Solution ph is 8.0 ~ 9.5.
Principle of the present invention is that Complexing Iron desulfurizing agent adopts alkaline solution absorption hydrogen sulfide gas to generate HS in absorption process
-, pass through Fe
3+l is by HS
-be oxidized to sulphur simple substance, simultaneously Fe
3+l is reduced to Fe
2+l; At regenerative process Fe
2+l is oxidized to Fe again by the oxygen in air
3+l, desulfurizing agent is regenerated, cyclic absorption hydrogen sulfide gas.Its key reaction is as follows:
(1) H
2the absorption oxidation of S
H
2S(aq)→H
++HS
-
HS
-+2Fe
3+L
n-→2Fe
2+L
n-+2H
++S↓
(2) Fe
2+oxidation regeneration
O
2(aq)+4Fe
2+L
n-+2H
2O→4Fe
3+L
n-+4OH
-
Beneficial effect of the present invention:
The present invention is a kind of novel process removing hydrogen sulfide combined with high-gravity technology by novel Complexing Iron desulfurizing agent.The desulfurizing agent desulfuration efficiency of this technique is high (single absorbs after cure hydrogen concentration lower than 10ppm), work Sulfur capacity high (can 1.35g/L be reached), Complexing Iron desulfurizing agent stablizes (total concentration of iron can reach 12g/L), sulfur granules free settling (sedimentation sulphur particle diameter concentrated on 140 ~ 177 microns in 3 ~ 8 minutes); The high-gravity technology gas-liquid mass transfer efficiency of this technique is high, liquid circulation amount is few, floor space is little, and whole equipment can skid.Thus reduction equipment investment, reduce energy consumption, give full play to the significant advantage that novel Complexing Iron desulfurizing agent combines with high-gravity technology.
Accompanying drawing explanation
Fig. 1 is process chart of the present invention.
In figure, 1 is fluid reservoir, and 2 is desulfurization cross_flow rotating packed bed, and 3 is regeneration cross_flow rotating packed bed, and 4 is filter, and 5 is H 2 S-containing gas, and 6 is Purge gas, and 7 is air, and 8 is air-discharging, and 9 is solid sulfur.
Detailed description of the invention
Further illustrate the present invention below by embodiment, but be not limited to following examples.
First, the example of compound sulfur granules sedimentation agent is as follows:
Example a: sulfur granules sedimentation agent, is made up of following ingredients: decyl alcohol 50mg/L, hexadecanol 40mg/L, PAM4mg/L, shitosan 10mg/L, sublimed sulfur 10mg/L, sodium metasilicate 35mg/L;
Example b: sulfur granules sedimentation agent, is made up of following ingredients: decyl alcohol 24mg/L, hexadecanol 96mg/L, polyglycol ether 30mg/L, sublimed sulfur 30mg/L, aluminium chloride 50mg/L;
Example c: sulfur granules sedimentation agent, is made up of following ingredients: aluminium chloride 10mg/L, polyglycol ether 50mg/L, shitosan 5mg/L, sublimed sulfur 10mg/L, PAM10mg/L, sodium metasilicate 15mg/L;
Example d: sulfur granules sedimentation agent, is made up of following ingredients: decyl alcohol 96mg/L, hexadecanol 24mg/L, polyglycol ether 80mg/L, PAM4mg/L, shitosan 40mg/L, sublimed sulfur 10mg/L, sodium metasilicate 5mg/L, aluminium chloride 80mg/L;
Example e: sulfur granules sedimentation agent, is made up of following ingredients: decyl alcohol 60mg/L, hexadecanol 60mg/L, shitosan 10mg/L, sublimed sulfur 10mg/L, PAM4mg/L, sodium metasilicate 5mg/L.
Secondly, the example of multi-functional corrosion inhibior is as follows:
Example a: Sodium Benzoate 0.2g/L, potassium sulfate 1g/L, sodium tungstate 0.1g/L, potassium silicate 0.2g/L, KBr 0.5g/L, formaldehyde 1g/L, dodecyl sodium sulfate 0.2g/L
Example b: Sodium Benzoate 0.2g/L, sodium sulphate 1.6g/L, sodium tungstate 0.1g/L, potassium silicate 0.2g/L, KBr 0.5g/L, formaldehyde 1g/L, dodecyl sodium sulfate 0.2g/L
Example c: Sodium Benzoate 1g/L, sodium sulphate 6g/L, sodium tungstate 0.3g/L, potassium silicate 1g/L, KBr 2g/L, formaldehyde 3.5g/L, paratoluenesulfonic acid sodium salt 1g/L
Example d: Sodium Benzoate 2g/L, potassium sulfate 8g/L, sodium tungstate 0.5g/L, potassium silicate 1g/L, KI 5g/L, formaldehyde 5g/L, paratoluenesulfonic acid sodium salt 2g/L
Embodiment 1: the preparation method of Complexing Iron desulfurizing agent:
Become total concentration of iron to be the solution of 2.2g/L according to the proportions that mol ratio is 3:1:1.2:3.6 ammonium ferric sulfate, iron ammonium sulfate, citric acid, HEDTA, in solution, add Na
2cO
319g/L, Sodium Benzoate 1.3g/L, compound sulfur granules sedimentation agent example a:0.15g/L, multi-functional corrosion inhibior example b:0.4g/L make Complexing Iron desulfurizing agent;
Embodiment 2: the preparation method of Complexing Iron desulfurizing agent:
Become total concentration of iron to be the solution of 7g/L according to the proportions that mol ratio is 3:2:1:6:1.2 ammonium ferric sulfate, ferric sulfate, iron ammonium sulfate, NTA, HEDTA, in solution, add NaOH and Na
2cO
3complexing Iron desulfurizing agent is made Deng mixture 35g/L, the mixture 4.6g/L of the mass ratio such as Sodium Benzoate and sodium thiosulfate of mass ratio, compound sulfur granules sedimentation agent example c:0.66g/L, multi-functional corrosion inhibior example d:1.3g/L;
Embodiment 3: the preparation method of Complexing Iron desulfurizing agent:
Become total concentration of iron to be the solution of 12g/L according to the proportions that mol ratio is 2:1:1:1:3.6 ammonium ferric sulfate, ferric sulfate, iron ammonium sulfate, gluconic acid, NTA, in solution, add KOH and K
2cO
3complexing Iron desulfurizing agent is made Deng mixture 48g/L, the imidazoles 7.2g/L of mass ratio, compound sulfur granules sedimentation agent example e:1.1g/L, multi-functional corrosion inhibior example c:3.4g/L;
Embodiment 4: the using method of Complexing Iron desulfurizing agent
As shown in Figure 1: remove the hydrogen sulfide in gas with novel Complexing Iron desulfurizing agent of the present invention, Complexing Iron desulfurizing agent in fluid reservoir 1 is pumped into desulfurization cross_flow rotating packed bed 2 and H 2 S-containing gas 5 counter current contacting in the filler of rotary drum, the alkaline solution absorption that H 2 S-containing gas 5 is desulfurized in agent is converted into HS
-, be desulfurized the Fe in agent
3+l is oxidized to sulphur simple substance, the Fe in desulfurizing agent
3+l is reduced to Fe
2+l; Remove the Purge gas after hydrogen sulfide 6 emptying after the built-in demister of cross_flow rotating packed bed, Complexing Iron sulfur removing pregnant solution pumps into regeneration cross_flow rotating packed bed 3 and air 7 cross-flow or counter current contacting in the filler of rotary drum, the Fe in desulfurizing agent
2+l is oxidized to Fe again by the oxygen in air
3+l; Desulfurizing agent after regeneration is pumped in fluid reservoir 1, add compound sulfur granules sedimentation agent, make sulphur rapid flocculation be deposited to bottom fluid reservoir 1, then pump in filter 4, the sulphur cake formed carries out subsequent treatment, and filtrate carries out next circulation desulfurization process getting back to fluid reservoir 1.
(1) experiment condition
Be the experimental gas of 1300ppm by natural gas formulating vulcanization hydrogen concentration.
Experimental gas flow: 2Nm
3/ h
Experimental liquid flow: 20L/h
Absorption, regeneration temperature: 40 ~ 50 DEG C
Solution ph: 8.5
(2) desulfurized effect
| Premature cure hydrogen concentration/ppm | Purified gas concentration of hydrogen sulfide/ppm | Desulfurization degree/% | |
| Desulfurizing agent 1 | 1300 | 0.5 | 99.92 |
| Desulfurizing agent 2 | 1300 | 0 | 100 |
| Desulfurizing agent 3 | 1300 | 0 | 100 |
Embodiment 5: the using method of Complexing Iron desulfurizing agent
Test method is with embodiment 4
(1) experiment condition
Be the experimental gas of 6000ppm by coking dry gas formulating vulcanization hydrogen concentration.
Experimental gas flow: 2Nm
3/ h
Experimental liquid flow: 60L/h
Absorption, regeneration temperature: 40 ~ 50 DEG C
Solution ph: 8.5
(2) desulfurized effect
| Premature cure hydrogen concentration/ppm | Purified gas concentration of hydrogen sulfide/ppm | Desulfurization degree/% | |
| Desulfurizing agent 1 | 6000 | 9 | 99.85 |
| Desulfurizing agent 2 | 6000 | 5 | 99.92 |
| Desulfurizing agent 3 | 6000 | 3 | 99.95 |
Embodiment 6: the using method of Complexing Iron desulfurizing agent
Test method is with embodiment 4
(1) experiment condition
Be the experimental gas of 10000ppm by water-gas formulating vulcanization hydrogen concentration.
Experimental gas flow: 2Nm
3/ h
Experimental liquid flow: 80L/h
Absorption, regeneration temperature: 40 ~ 50 DEG C
Solution ph: 8.5
(2) desulfurized effect
| Premature cure hydrogen concentration/ppm | Purified gas concentration of hydrogen sulfide/ppm | Desulfurization degree/% | |
| Desulfurizing agent 1 | 10000 | 10 | 99.90 |
| Desulfurizing agent 2 | 10000 | 9 | 99.91 |
| Desulfurizing agent 3 | 10000 | 5.5 | 99.95 |
Claims (8)
1. a Complexing Iron desulfurizing agent, is characterized in that: be made up of following component: soluble ferric iron salt, molysite chelating agent, sulphur compound absorbent, stabilizing agent, compound sulfur granules sedimentation agent and multi-functional corrosion inhibior; Fe is contained in soluble ferric iron salt in desulfurizing agent
3+with Fe
2+mol ratio be 1:3 ~ 5:1; The mol ratio of chelating agent and molysite is 1.2:1 ~ 3:1; Solution ph is 8.0 ~ 9.5; Each component proportion is as follows:
Soluble ferric iron salt: 2.2 ~ 12 parts,
Molysite chelating agent: 5 ~ 20 parts;
Sulphur compound absorbent: 15 ~ 70 parts;
Stabilizing agent: 0.1 ~ 15 part;
Compound sulfur granules sedimentation agent: 0.05 ~ 2 part;
Multi-functional corrosion inhibior: 0.05 ~ 5 part.
2. Complexing Iron desulfurizing agent according to claim 1, is characterized in that: containing Fe in described soluble ferric iron salt
3+with Fe
2+, wherein provide Fe
3+be FeNH
4(SO
4)
212H
2o or Fe
2(SO
4)
3in at least one, wherein provide Fe
2+be Fe
2(NH
4)
2(SO
4)
26H
2o.
3. Complexing Iron desulfurizing agent according to claim 1, is characterized in that: described chelating agent is EDTA, Na
4eDTA, NTA, Na
3nTA, HEDTA, Na
3one or more in HEDTA, DTPA, HEDP, TEA, citric acid, natrium citricum, sulfosalicylic acid, sulfosalicylic acid sodium salt, gluconic acid.
4. Complexing Iron desulfurizing agent according to claim 1, is characterized in that: described sulphur compound absorbent is NaOH, Na
2cO
3, NaHCO
3, KOH, K
2cO
3, KHCO
3in one or more.
5. Complexing Iron desulfurizing agent according to claim 1, is characterized in that: described stabilizing agent is one or more in imidazoles, benzoate, alkali metal chlorizated salt, alkali metal thiosulfate.
6. Complexing Iron desulfurizing agent according to claim 1, is characterized in that: described compound sulfur granules sedimentation agent is made up of the initator that flocculates, flocculation flocculating agent, flocculating setting agent:
Described flocculation initator is one or both in sublimed sulfur, shitosan, and content is 12% ~ 20% of sulfur granules sedimentation agent;
Described flocculation flocculating agent is AlCl
3, one or both in sodium metasilicate, content is 3% ~ 32% of sulfur granules sedimentation agent;
Described flocculating setting agent is two or more in PAM, straight chain decyl alcohol, polyglycol ether, straight chain hexadecanol, and content is 55% ~ 84% of sulfur granules sedimentation agent.
7. Complexing Iron desulfurizing agent according to claim 1, is characterized in that: described multi-functional corrosion inhibior helps corrosion inhibiter, antibacterial type corrosion inhibiter, stable potential corrosion inhibiter to form by the main corrosion inhibiter of stable complexation iron, stable complexation iron:
Described main corrosion inhibiter is one or more the mixture in alkali metal sulfates, tungstates, and content is 27% ~ 57% of multi-functional corrosion inhibior;
The described corrosion inhibiter that helps is one or more mixture in alkali metal benzoate, silicate, and content is 3% ~ 15% of multi-functional corrosion inhibior;
Described antibacterial type corrosion inhibiter is one or more the mixture in KBr, KI, formaldehyde, and content is 18% ~ 66% of multi-functional corrosion inhibior;
Described stable potential corrosion inhibiter is one or both in dodecyl sodium sulfate, paratoluenesulfonic acid sodium salt, and content is 3% ~ 11% of multi-functional corrosion inhibior.
8. a using method for the Complexing Iron desulfurizing agent described in any one of claim 1 ~ 7, is characterized in that: comprise the following steps:
(1) the Complexing Iron desulfurizing agent in fluid reservoir is pumped into desulfurization cross_flow rotating packed bed and gas flow for 2Nm with the flow of 20 ~ 80L/h
3/ h H 2 S-containing gas is counter current contacting in the filler of rotary drum, and the alkaline solution absorption that hydrogen sulfide gas is desulfurized in agent is converted into HS
-, be desulfurized the Fe in agent
3+l is oxidized to sulphur simple substance, the Fe in desulfurizing agent
3+l is reduced to Fe
2+l, absorbing temperature is 40 ~ 50 DEG C;
(2) remove the gas after hydrogen sulfide emptying after the built-in demister of cross_flow rotating packed bed, Complexing Iron sulfur removing pregnant solution pumps into regeneration cross_flow rotating packed bed and air counter current contacting in the filler of rotary drum with the flow of 20 ~ 80L/h, the Fe in desulfurizing agent
2+l is oxidized to Fe again by the oxygen in air
3+l, regeneration temperature is 40 ~ 50 DEG C;
(3) desulfurizing agent after regeneration is pumped in fluid reservoir, add compound sulfur granules sedimentation agent, make sulphur rapid flocculation be deposited to bottom reservoir, then pump in filter, the sulphur cake formed carries out subsequent treatment, and filtrate returns fluid reservoir and carries out next circulation desulfurization process.
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