CN103878029B - A kind of supplements-iron for complex iron desulphurization solution and preparation method thereof - Google Patents
A kind of supplements-iron for complex iron desulphurization solution and preparation method thereof Download PDFInfo
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- CN103878029B CN103878029B CN201410048821.2A CN201410048821A CN103878029B CN 103878029 B CN103878029 B CN 103878029B CN 201410048821 A CN201410048821 A CN 201410048821A CN 103878029 B CN103878029 B CN 103878029B
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- Prior art keywords
- iron
- supplements
- complex
- preparation
- complexing agent
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 117
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 68
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 229910052751 metal Inorganic materials 0.000 claims abstract 2
- 239000002184 metal Substances 0.000 claims abstract 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 239000008139 complexing agent Substances 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 7
- -1 Hedta (HEDTA) Chemical compound 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 2
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 2
- 230000000536 complexating effect Effects 0.000 claims description 2
- KYQODXQIAJFKPH-UHFFFAOYSA-N diazanium;2-[2-[bis(carboxymethyl)amino]ethyl-(carboxylatomethyl)amino]acetate Chemical compound [NH4+].[NH4+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O KYQODXQIAJFKPH-UHFFFAOYSA-N 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 claims description 2
- 150000007524 organic acids Chemical class 0.000 claims description 2
- 150000007529 inorganic bases Chemical class 0.000 claims 2
- 230000007797 corrosion Effects 0.000 abstract description 5
- 238000005260 corrosion Methods 0.000 abstract description 5
- 150000003839 salts Chemical class 0.000 abstract description 5
- 239000012535 impurity Substances 0.000 abstract description 4
- 239000003513 alkali Substances 0.000 abstract description 3
- 238000004065 wastewater treatment Methods 0.000 abstract description 3
- 238000002425 crystallisation Methods 0.000 abstract description 2
- 230000008025 crystallization Effects 0.000 abstract description 2
- 239000002738 chelating agent Substances 0.000 abstract 1
- 238000006477 desulfuration reaction Methods 0.000 description 14
- 230000023556 desulfurization Effects 0.000 description 9
- 150000001450 anions Chemical class 0.000 description 8
- 238000003756 stirring Methods 0.000 description 7
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 241000370738 Chlorion Species 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 description 2
- 229910000360 iron(III) sulfate Inorganic materials 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical class [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000011790 ferrous sulphate Substances 0.000 description 1
- 235000003891 ferrous sulphate Nutrition 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 235000000396 iron Nutrition 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 229910021653 sulphate ion Inorganic materials 0.000 description 1
- 230000000153 supplemental effect Effects 0.000 description 1
- 230000009469 supplementation Effects 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
Landscapes
- Treatment Of Water By Oxidation Or Reduction (AREA)
- Removal Of Specific Substances (AREA)
Abstract
The present invention relates to replenishers of iron and preparation method thereof in a kind of complex iron desulphurization solution.By the hydrous oxide (Fe of iron
xo
yh
2o) react under uniform temperature condition with metal chelating agent and alkali and prepare.Compared with conventional supplements-iron, because it is not containing such as Cl
-, NO
3 -, SO
4 2-deng impurity cloudy from, therefore effectively eliminate Cl
-the equipment corrosion problem caused, also eliminates by NO
3 -the subsequent wastewater treatment problem caused, is priorly that it avoids due to SO
4 2-the crystallization of the salt that enrichment brings, significantly can reduce the loss of doctor solution and the safe operation of equipment.
Description
Technical field
The present invention relates to the preparation method of environment protection desulphurization field catalyst, be specifically related to replenishers of iron and preparation method thereof in complex iron desulfurization.
Background technology
Complex iron desulfur technology has been widely used in oil plant, gas plant and sewage treatment plant to containing H
2the waste gas of S carries out processing and it being converted into sulphur, to reach the requirement of environment protection emission.Complex iron desulfur technology uses a kind of complex iron desulphurization solution of interworking type, in this desulfuration solution, play desulfidation be wherein with complex pattern exist iron, its reaction principle is as follows:
H
2S+NaOH→Na
++HS
－+H
2O
HS
-+ 2Fe
3+(complex state) → 2Fe
2+(complex state)+H
++ S ↓
1/2O
2(in solution)+H
2o+2Fe
2+(complex state) → 2OH
-+ 2Fe
3+(complex state)
Total desulphurization reaction:
H
2S+1/2O
2→S+H
2O
Because complex iron desulphurization solution iron in regenerative process consumes because instability meeting is continuous, and such as sulfate radical, inferior sulfate radical, thiosulfate anion, nitrate anion, chlorion or other anion accumulative in desulfuration solution, need when exceeding finite concentration scope to take out a part of desulfuration solution in time, these factors can cause the concentration of iron ion in doctor solution constantly to reduce, thus reduce desulfurization performance.In order to maintain the enough total iron contents of doctor solution, continuous supplementation in actual application, is needed to have the iron ion of desulphurizing activated complex status.Supplemented these active irons, source of iron selects the molysite of solubility usually in the past.Soluble-salt mainly iron chloride, ferric nitrate or sulfuric acid (Asia) iron of iron.As US Patent No. 4009251 adopts iron chloride, ferric sulfate to add in doctor solution as source of iron; European patent EP 0107213 adopts ferric nitrate as source of iron; Chinese patent CN101874968 adopts iron chloride, ferric sulfate, ferrous sulfate as the complementary element of iron.
FeCl
3+ complexing agent → Fe
3+(complex state)+3Cl
-
Fe (NO
3)
3+ complexing agent → Fe
3+(complex state)+3NO
3 -
Fe
2(SO
4)
3+ complexing agent → 2Fe
3+(complex state)+3SO
4 2-
Because chlorion is serious to equipment corrosion, when selecting iron chloride to carry out supplementary as source of iron, usually comparatively harsh to the selection of equipment, thus cause whole environment protection desulphurization construction costs expensive; And when selecting ferric nitrate, although equipment corrosion is alleviated to some extent, require higher to follow-up wastewater treatment, because wherein need to process containing a large amount of ammonia nitrogens; Select sulfuric acid (Asia) iron as source of iron, relative nitrate, the solubility of sulfate is lower, therefore be accumulated to when to a certain degree and not processing, there will be sulphate crystal in desulphurization system, desulphurization system time serious, can be caused normally to run, therefore needing when taking sulfate as source of iron a large amount of outer row's desulfuration solution to reach reasonable level with the concentration maintaining salt, but the desulfuration solution discharge of costliness can increase the burden of desulfurization enterprise, very uneconomical.From actual motion effect, no matter take which kind of soluble ferric iron salt above as the supplemental components of iron, after adding salt, namely above-mentioned impurity anions is stayed in doctor solution, the existence of these ions can produce " ionic effect ", will affect the desulphurizing activated of Complexing Iron doctor solution.
For this reason, the invention provides and a kind ofly add not containing the supplements-iron of above impurity anions the enrichment that this supplements-iron can not cause anion, namely overcome equipment corrosion, the deficiency of doctor solution loss that the precipitation that simultaneously turn avoid salt causes.
Summary of the invention
The object of the invention is to solve existing supplements-iron and contain the deficiency that a large amount of objectionable impurities anion causes, provide one not containing Cl
-, NO
3 -, SO
4 2-supplements-iron of anion and preparation method thereof.
Technical scheme of the present invention:
The preparation method of the supplements-iron of described anion free from foreign meter, can adopt following raw material and be prepared from the steps below:
1. main material is the hydrous oxide of iron, its chemical formula Fe
xo
yh
2o represents, the chemical valence of iron (comprises 2 and 3) between 2 ~ 3.
2. main material is organic acid complexing agent, selects one or more the combination in b diammonium edta (EDTA), Hedta (HEDTA), diethylenetriamine pentacarboxylic acid (DTPA), nitrilotriacetic acid (NTA).
Preparation process: (1) is by appropriate Fe
xo
yh
2o, complexing agent, alkali and deionized water join in the reactor with heating agitating function successively, and be warmed up to 50 ~ 100 DEG C, stirring reaction 3 ~ 5 hours, obtains dark red-brown liquid, be supplements-iron.Alkali used is NaOH or KOH.
Compared with prior art, this technology tool has the following advantages:
Owing to not containing such as Cl in this doctor solution
-, NO
3 -, SO
4 2-deng acid ion, the enrichment of anion can not be produced, avoid the crystallization of salt in solution; The equipment of avoiding suffers serious corrosion, and under similarity condition, equipment selection is more extensive, can select the material of cheaper; Wastewater treatment is also easier.
Detailed description of the invention
Following examples are further describing process of the present invention.
Embodiment 1
550Kg deionized water is added successively, 790KgEDTA, 100KgFe in stirred tank
2o
3h
2o, in reactor, then add NaOH regulate between pH value 7 ~ 9, be warmed up to 50 DEG C, stirring reaction 3 hours, obtains supplements-iron, and analysis total iron content is wherein at 58g/L.The desulfurization performance of this supplements-iron is shown in Table 1.
Embodiment 2
950Kg deionized water is added successively, 400KgEDTA, 100KgFe in stirred tank
2o
3h
2o, in reactor, then add NaOH regulate between pH value 7 ~ 9, be warmed up to 80 DEG C, stirring reaction 4 hours, obtains supplements-iron, and analysis total iron content is wherein at 57g/L.The desulfurization performance of this supplements-iron is shown in Table 1.
Embodiment 3
980Kg deionized water is added successively, 665KgHEDTA, 100KgFe in stirred tank
2o
3feOH
2o, in reactor, then add KOH regulate between pH value 7 ~ 9, be warmed up to 60 DEG C, stirring reaction 5 hours, obtains supplements-iron, and analysis total iron content is wherein at 50g/L.The desulfurization performance of this supplements-iron is shown in Table 1.
Embodiment 4
900Kg deionized water is added successively, 460KgDTPA, 50KgFe in stirred tank
2o
3h
2o and 50KgFe
2o
3feOH
2o, in reactor, then add KOH regulate between pH value 7 ~ 9, be warmed up to 100 DEG C, stirring reaction 5 hours, obtains supplements-iron, and analysis total iron content is wherein at 60g/L.The desulfurization performance of this supplements-iron is shown in Table 1.
Embodiment 5
750Kg deionized water is added successively, 450KgNTA, 100KgFe in stirred tank
2o
3h
2o, in reactor, then add NaOH regulate between pH value 7 ~ 9, be warmed up to 70 DEG C, stirring reaction 3 hours, obtains supplements-iron, and analysis total iron content is wherein at 55g/L.The desulfurization performance of this supplements-iron is shown in Table 1.
Embodiment 6
550Kg deionized water is added successively, 400KgEDTA, 200KgNTA, 100KgFe in stirred tank
2o
3h
2o, in reactor, then add KOH regulate between pH value 7 ~ 9, be warmed up to 90 DEG C, stirring reaction 4 hours, obtains supplements-iron, and analysis total iron content is wherein at 56g/L.The desulfurization performance of this supplements-iron is shown in Table 1.
The desulphurizing activated test of table 1 supplements-iron
Claims (1)
1. for a preparation method for the supplements-iron of complex iron desulphurization solution, it is characterized in that: comprise the following steps:
Deionized water, source of iron, complexing agent are joined in reactor, with inorganic base adjust pH to 7 ~ 9, within 3 ~ 5 hours, obtains reddish brown viscous liquid 50 ~ 100 DEG C of reactions, be supplements-iron; Wherein:
Described supplements-iron is not containing Cl
-, NO
3 -, SO
4 2-ion,
The hydrous oxide using iron is source of iron,
Use the organic acid with metal complexing capability as complexing agent;
The composition Fe of source of iron
xo
yh
2o represents, the chemical valence of iron is not less than 2 and not higher than 3;
Complexing agent is one or more in b diammonium edta (EDTA), Hedta (HEDTA), diethylenetriamine pentacarboxylic acid (DTPA), nitrilotriacetic acid (NTA), and the mol ratio of complexing agent and iron is (1 ~ 2): 1;
Inorganic base is NaOH or potassium hydroxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410048821.2A CN103878029B (en) | 2014-02-12 | 2014-02-12 | A kind of supplements-iron for complex iron desulphurization solution and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410048821.2A CN103878029B (en) | 2014-02-12 | 2014-02-12 | A kind of supplements-iron for complex iron desulphurization solution and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN103878029A CN103878029A (en) | 2014-06-25 |
| CN103878029B true CN103878029B (en) | 2016-02-03 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107353929A (en) * | 2017-07-18 | 2017-11-17 | 付增华 | A kind of desulfurizing agent and its application |
| CN113578391B (en) * | 2021-08-11 | 2023-10-27 | 四川炳辉环保科技有限责任公司 | Wet liquid phase desulfurization catalyst and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101134918A (en) * | 2006-08-28 | 2008-03-05 | 北京三聚环保新材料有限公司 | Desulfurizer active component having high sulfur-content and preparation method thereof |
| CN101327397A (en) * | 2008-07-03 | 2008-12-24 | 大连理工大学 | Method for simultaneously removing SO2 and NO in flue gas by biological reduction and complexing absorption |
| CN101874968A (en) * | 2009-12-31 | 2010-11-03 | 中北大学 | Iron complex desulfurizer suitable for super-gravity desulfurization |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4869543B2 (en) * | 2003-01-31 | 2012-02-08 | 新日本製鐵株式会社 | Wastewater purification method |
-
2014
- 2014-02-12 CN CN201410048821.2A patent/CN103878029B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101134918A (en) * | 2006-08-28 | 2008-03-05 | 北京三聚环保新材料有限公司 | Desulfurizer active component having high sulfur-content and preparation method thereof |
| CN101327397A (en) * | 2008-07-03 | 2008-12-24 | 大连理工大学 | Method for simultaneously removing SO2 and NO in flue gas by biological reduction and complexing absorption |
| CN101874968A (en) * | 2009-12-31 | 2010-11-03 | 中北大学 | Iron complex desulfurizer suitable for super-gravity desulfurization |
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| CN103878029A (en) | 2014-06-25 |
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Denomination of invention: An iron supplement for complex iron desulfurization solution and its preparation method Effective date of registration: 20230330 Granted publication date: 20160203 Pledgee: Industrial Bank Co.,Ltd. Yinchuan Branch Pledgor: NINGXIA SHENGLAN CHEMICAL ENVIRONMENTAL PROTECTION TECHNOLOGY Co.,Ltd. Registration number: Y2023980036999 |
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