CN1539545A - Iterative regenerable desulfurizer and producing method - Google Patents
Iterative regenerable desulfurizer and producing method Download PDFInfo
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- CN1539545A CN1539545A CNA2003101016954A CN200310101695A CN1539545A CN 1539545 A CN1539545 A CN 1539545A CN A2003101016954 A CNA2003101016954 A CN A2003101016954A CN 200310101695 A CN200310101695 A CN 200310101695A CN 1539545 A CN1539545 A CN 1539545A
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Abstract
A ocyclically regenerated desulfurizing agent for removing hydrogen sulfide and organic sulfur is prepared from iron oxide or sponge iron, adhesive, oxide of alkali metal-alkali earth metal, pore-forming agent and synergist through pre-treating, immersing, kneading, shaping, calcining and activating. Its advantage is wide temp range.
Description
Technical field:
The present invention relates to the desulfurizing agent technical field, particularly the iterative regenerable desulfurizer technical field.
Background technology:
In oil refining, chemical industry and the natural gas production process, the existence meeting of hydrogen sulfide brings to ordinary production and seriously influences.Hydrogen sulfide not only has corrosiveness to pipeline, equipment.Hydrogen sulfide also can make catalyst poisoning, and what influence was produced normally carries out.In addition, hydrogen sulfide gas has very strong toxicity, and the discharging meeting works the mischief to environment and people and animals.At present, remove hydrogen sulfide several different methods is arranged.The fixed bed desulfurizing agent mainly contains zinc oxide, active carbon and ferric oxide desulfurizer.The common serviceability temperature of Zinc oxide desulfurizer is 200-500 ℃, and at this moment the effect of Zinc oxide desulfurizer is better.Though also be useful on the zinc oxide of low temperature, effect is unsatisfactory, (9%W/W) is less for its Sulfur capacity.Activated carbon desulphurization agent can be regenerated, but its intensity is relatively poor, easily produces the fine powder blocking pipe.Ferric oxide desulfurizer is more and more extensively cognitive by people as a kind of ancient desulfurizing agent.
Patent CN1354307A discloses a kind of iron oxide compound desulfurizer.This desulfurizing agent iron one zinc is composite desulfurizing agent.Have characteristics such as Sulfur capacity height, cost are low, but its serviceability temperature is higher,, does not investigate during normal temperature greater than using more than 200 ℃.
Patent CN1121950A discloses a kind of dry shaping desulfurizing agent and preparation and purposes.Its active component is natural iron ore, iron ore slag and zinc oxide, is adding entry, pore creating material, binding agent etc., forms through mixing extrusion.Be characterized in that production cost is low, at normal temperatures and pressures, remove the efficient height of hydrogen sulfide, anti-carbon dioxide content advantages of higher, but it is non-renewable.
Growing along with modern times oil refining, chemical process, people have proposed more and more higher requirement to the performance of desulfurizing agent.Except require desulfurizing agent have higher degree of purification (＜1ppm), bigger sulfur capacity, preferably the water resistance, also require desulfurizing agent to have functions such as certain denitrogenation, desulfurization.
Patent CN1074685C discloses a kind of desulfurizing agent and preparation method thereof.This desulfurizing agent is with Ca
2Fe
2O
5Desulfurizing agent for active component.This desulfurizing agent is mixed with the powder of iron oxide/iron hydroxide/ferric nitrate powder and calcium oxide/calcium hydroxide/calcium carbonate/calcium bicarbonate, wherein the mol ratio of iron and calcium is 1: 1 to 1: 5, compound is added water stir, extruded moulding, roasting forms under the 700-1100 ℃ of following oxidizing atmosphere.Its characteristics are the Sulfur capacity height, and serviceability temperature wide ranges (5-100 ℃) purifies thoroughly (outlet silver nitrate detect less than).Though it is renewable to mention bubbling air, the mode of regeneration does not mention in detail that the desulfurized effect after the regeneration is not seen description yet.
Summary of the invention:
Technical problem solved by the invention has provided a kind of desulfurizing agent of iterative regenerable, this desulfurizing agent except have higher sulfur capacity, higher desulfurized effect, preferably intensity, the good resistance to water, having simultaneously is reusable performance at bubbling air simply.
The invention provides the preparation method of the desulfurizing agent of producing this kind iterative regenerable simultaneously, this kind preparation method technology is simple, and is easy and simple to handle.
For achieving the above object, the technical solution used in the present invention is: a kind of iterative regenerable desulfurizer, this iterative regenerable desulfurizer contains iron oxide or the sponge iron of mass ratio 20-80%, the binding agent of mass ratio 0-30%, alkali metal-alkaline earth oxide of mass ratio 10-80%, the pore creating material of mass ratio 1-10%, mass ratio 1-5% synergist;
One or more of binding agent are carclazyte, kaolin, bentonite etc.;
One or more of alkali metal-alkaline earth oxide are oxide, hydroxide and carbonate thereof or the nitrate of sodium, potassium, magnesium, calcium;
One or more of pore creating material are carbon dust, starch, carbon ammonium, wood chip etc.;
Synergist is an oxygenatedchemicals;
The preparation method of the desulfurizing agent of iterative regenerable:
1) adding water mixes: with iron oxide or the sponge iron of mass ratio 15-80%, the binding agent of mass ratio 0-30%, alkali metal-alkaline earth oxide of mass ratio 10-80%, the pore creating material of mass ratio 1-10%, mass ratio 1-5% synergist add water and mix;
2) moulding;
3) dry or dry;
4) roasting: be under 500-1000 ℃ the condition in temperature, roasting 0.5-8 hour;
5) activation: the desulfurizing agent after the roasting is soaked in alkali-metal hydroxide or its carbonate solution, and the time is 0.5-8 hour; Desulfurizing agent after soaking is carried out saturated processing under carbon dioxide atmosphere, the time is that acid solution is a mineral acid solution, or organic acidity solution;
Mineral acid solution is hydrochloric acid, sulfuric acid, nitric acid, the hypochlorous aqueous solution;
In the air speed scope is 0.5～10 hour
-1, 0～150 ℃ of temperature conditions use down.
Owing to adopted technical scheme provided by the present invention, made stability improver and manufacture method thereof that this kind provided by the present invention is used in the refining of petroleum products process produce following beneficial effect:
Because what the present invention adopted is binding agent and catalytic cracking spent catalyst, with low cost; Desulfurization, nitric efficiency height remove nitride and sulfide in the oil product, significantly improve the stability of oil product.
The specific embodiment 1:
Select binding agent carclazyte 10 grams for use, specific area is 240 meters
2Catalytic cracking spent catalyst 90 grams of/gram; Add 500 ml concns and carry out preliminary treatment: stirred 4 hours down at 30 ℃ for 1M watery hydrochloric acid; After the filtration, obtain pretreated carclazyte-dead catalyst mixture; Kneading at room temperature, moulding, dry; 550 ℃ of roasting temperatures 2 hours, light grey stability improver.
Getting the above-mentioned stability improver that makes of 1.0 grams is in the acid buret of 50ml in volume, and adding temperature continuously in buret is 42 ℃, and colourity is 8 diesel oil 1000ml, and control diesel oil is 1 hour by the air speed of modifier
-1The about 1000ml of the diesel oil that obtains making with extra care.The analysis showed that the colourity of refining back diesel oil is 1.5.
The refined diesel oil that obtains is stored in respectively in the sealing Brown Glass Brown glass bottles and jars only, and lucifuge was deposited 30 days under the room temperature, surveyed its colourity 1.5.
This stability improver is with low cost; Desulfurization, nitric efficiency height remove nitride and sulfide in the oil product, significantly improve the stability of oil product.
The specific embodiment 2:
Select 20 gram kaolin for use, 80 gram specific surfaces are 215 meters
2The catalytic cracking spent catalyst of/gram; Add 300 ml concns and carry out preliminary treatment: stirred 2 hours down at 40 ℃ for 2M watery hydrochloric acid; After the filtration, obtain pretreated kaolin-dead catalyst mixture; Kneading at room temperature, moulding, oven dry; 650 ℃ of roasting temperatures 3 hours, light grey stability improver.
Getting the above-mentioned stability improver that makes of 1.0 grams is in the acid buret of 50ml in volume, and adding temperature continuously in buret is 60 ℃, and colourity is 8 diesel oil 1000ml, and control diesel oil is 1 hour by the air speed of modifier
-1The about 1000ml of the diesel oil that obtains making with extra care.The analysis showed that the colourity of refining back diesel oil is 1.0.
The refined diesel oil that obtains is stored in respectively in the sealing Brown Glass Brown glass bottles and jars only, and lucifuge was deposited 30 days under the room temperature, surveyed its colourity 1.0.
This stability improver is with low cost; Desulfurization, nitric efficiency height remove nitride and sulfide in the oil product, significantly improve the stability of oil product.
The specific embodiment 3:
Select 30 gram bentonites for use, 70 gram specific surfaces are 320 meters
2The catalytic cracking spent catalyst of/gram; Add 500 ml concns and carry out preliminary treatment: stirred 4 hours down at 40 ℃ for 6M watery hydrochloric acid; After the filtration, obtain 95 gram pretreated bentonite-dead catalyst mixtures; Kneading at room temperature, moulding, dry; 600 ℃ of roasting temperatures 1.5 hours, light grey stability improver 93 grams.
Getting the above-mentioned stability improver that makes of 1.0 grams is in the acid buret of 50ml in volume, and adding temperature continuously in buret is 80 ℃, and colourity is 8 diesel oil 1000ml, and control diesel oil is 1 hour by the air speed of modifier
-1The about 1000ml of the diesel oil that obtains making with extra care.The analysis showed that the colourity of refining back diesel oil is 0.5.
The refined diesel oil that obtains is stored in respectively in the sealing Brown Glass Brown glass bottles and jars only, and lucifuge was deposited 30 days under the room temperature, surveyed its colourity 0.5.
This stability improver is with low cost; Desulfurization, nitric efficiency height remove nitride and sulfide in the oil product, significantly improve the stability of oil product.
The specific embodiment 4:
Select 5 gram bentonites for use, 90 gram specific surfaces are 286 meters
2The catalytic cracking spent catalyst of/gram; Add 500 ml concns and carry out preliminary treatment: stirred 4 hours down at 40 ℃ for 6M watery hydrochloric acid; After the filtration, obtain pretreated bentonite-dead catalyst mixture; Kneading at room temperature, moulding, dry; 600 ℃ of roasting temperatures 1.5 hours, light grey stability improver.
Getting the above-mentioned stability improver that makes of 1.0 grams is in the acid buret of 50ml in volume, and adding temperature continuously in buret is 15 ℃, and colourity is 8 diesel oil 1000ml, and control diesel oil is 1 hour by the air speed of modifier
-1The about 1000ml of the diesel oil that obtains making with extra care.The analysis showed that the colourity of refining back diesel oil is 2.0.
The refined diesel oil that obtains is stored in respectively in the sealing Brown Glass Brown glass bottles and jars only, and lucifuge was deposited 30 days under the room temperature, surveyed its colourity 2.0.
This stability improver is with low cost; Desulfurization, nitric efficiency height remove nitride and sulfide in the oil product, significantly improve the stability of oil product.
The specific embodiment 5:
Select 5 gram carclazytes for use, 90 gram specific surfaces are 286 meters
2The catalytic cracking spent catalyst of/gram; Add 500 ml concns and carry out preliminary treatment: stirred 4 hours down at 40 ℃ for 6M watery hydrochloric acid; After the filtration, obtain pretreated bentonite-dead catalyst mixture; Kneading at room temperature, moulding, oven dry; 600 ℃ of roasting temperatures 1.5 hours, light grey stability improver.
Getting the above-mentioned stability improver that makes of 1.0 grams is in the acid buret of 50ml in volume, and adding temperature continuously in buret is 42 ℃, and colourity is 8 diesel oil 1000ml, and control diesel oil is 1 hour by the air speed of modifier
-1The about 1000ml of the diesel oil that obtains making with extra care.The analysis showed that the colourity of refining back diesel oil is 2.0.
The refined diesel oil that obtains is stored in respectively in the sealing Brown Glass Brown glass bottles and jars only, and lucifuge was deposited 30 days under the room temperature, surveyed its colourity 2.0.
This stability improver is with low cost; Desulfurization, nitric efficiency height remove nitride and sulfide in the oil product, significantly improve the stability of oil product.
Claims (8)
1, a kind of iterative regenerable desulfurizer, it is characterized in that: this iterative regenerable desulfurizer contains iron oxide or the sponge iron of mass ratio 15-80%, the binding agent of mass ratio 0-30%, alkali metal-alkaline earth oxide of mass ratio 15-80%, the pore creating material of mass ratio 1-10%, mass ratio 1-5% synergist.
2, the desulfurizing agent of iterative regenerable according to claim 1 is characterized in that: one or more of described binding agent are carclazyte, kaolin, bentonite etc.
3, the desulfurizing agent of iterative regenerable according to claim 1 is characterized in that: one or more of described alkali metal-alkaline earth oxide are oxide, hydroxide and carbonate thereof or the nitrate of sodium, potassium, magnesium, calcium.
4, the desulfurizing agent of iterative regenerable according to claim 1 is characterized in that: one or more of described pore creating material are carbon dust, starch, carbon ammonium, wood chip etc.
5, the desulfurizing agent of iterative regenerable according to claim 1 is characterized in that: described synergist is a transistion metal compound.
6, the preparation method of the desulfurizing agent of iterative regenerable according to claim 1:
1) adding water mixes: with iron oxide or the sponge iron of mass ratio 15-80%, the binding agent of mass ratio 0-30%, alkali metal-alkaline earth oxide of mass ratio 10-80%, the pore creating material of mass ratio 1-10%, mass ratio 1-5% synergist add water and mix;
2) moulding;
3) dry or dry;
4) roasting: be under 500-1000 ℃ the condition in temperature, roasting 0.5-8 hour;
5) activation: the desulfurizing agent after the roasting is soaked in alkali-metal hydroxide or its carbonate solution, and the time is 0.5-8 hour; Desulfurizing agent after soaking is carried out saturated processing under carbon dioxide atmosphere, the time is 0.5-8 days, gets the regenerating desulfurization agent.
7, the desulfurizing agent of iterative regenerable according to claim 1 is characterized in that: the desulfurizing agent air inversion regeneration of this iterative regenerable.
8, the desulfurizing agent of iterative regenerable according to claim 1 is characterized in that: regeneration back desulfurizing agent cleans with high temperature nitrogen, steam blowing or with carbon tetrachloride.
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7717979B2 (en) | 2006-08-28 | 2010-05-18 | Beijing Sj Environmental Protection And New Material Co., Ltd. | Composition for a desulfurizer with a high sulfur capacity and the process of making the same |
| CN101711925A (en) * | 2008-10-02 | 2010-05-26 | 巴斯夫欧洲公司 | Method for depletion of sulfur and/or compounds containing sulfur from a biochemically produced organic compound |
| CN101798625A (en) * | 2010-04-14 | 2010-08-11 | 北京科技大学 | Method for removing sulfur from fuel before sintering iron ores |
| CN101590396B (en) * | 2008-05-30 | 2012-02-15 | 北京三聚环保新材料股份有限公司 | Method for preparing and producing high-sulphur capacity iron-based desulfurizer |
| CN101584962B (en) * | 2008-05-23 | 2012-07-18 | 北京三聚环保新材料股份有限公司 | High-strength FeOOH desulfurizer and preparation method thereof |
| US8585993B2 (en) | 2008-12-30 | 2013-11-19 | Beijing Sanju Enviromental Protection and New Material Co., Ltd. | Method for regenerating amorphous iron oxide hydroxide and desulfurizer containing amorphous iron oxide hydroxide as active component |
| US8591847B2 (en) | 2008-12-30 | 2013-11-26 | Beijing Sanju Environmental Protection and New Material Co., Ltd. | Method for removing hydrogen sulfide from gaseous stream at normal temperature |
| US8603215B2 (en) | 2006-08-28 | 2013-12-10 | Beijing Sanju Environmental Protection and New Material Co., Ltd. | Composition of amorphous iron oxide hydroxide, desulfurizer comprising the same, and methods for preparing and regenerating the desulfurizer |
| US8647600B2 (en) | 2008-12-30 | 2014-02-11 | Beijing Sanju Environmental Protection and New Material Co., Ltd. | Methods for preparing and regenerating materials containing amorphous iron oxide hydroxide and desulfurizer comprising the same |
| US8652427B2 (en) | 2008-12-30 | 2014-02-18 | Beijing Sanju Environmental Protection and New Material Co., Ltd. | Preparation and repeated regeneration of material containing amorphous iron oxide hydroxide, desulfurization agents containing the material, and preparation and repeated regeneration thereof |
| CN104645951A (en) * | 2013-11-21 | 2015-05-27 | 东营科尔特化工科技有限公司 | Regeneration method of fine desulfuration agent of liquefied petroleum gas |
| CN105771620A (en) * | 2016-05-05 | 2016-07-20 | 张锐 | Efficient desulfurizer and preparation method thereof |
| CN106139880A (en) * | 2016-06-28 | 2016-11-23 | 安徽国能亿盛环保科技有限公司 | A kind of industrial waste gas desulfurizing agent and preparation method thereof |
| CN110564457A (en) * | 2019-07-26 | 2019-12-13 | 沈阳三聚凯特催化剂有限公司 | Deep purification fine desulfurizer and preparation method thereof |
| CN115093005A (en) * | 2022-06-27 | 2022-09-23 | 中节能工程技术研究院有限公司 | Waste alkali liquor oxidation desulfurization method |
-
2003
- 2003-10-28 CN CNA2003101016954A patent/CN1539545A/en active Pending
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8603215B2 (en) | 2006-08-28 | 2013-12-10 | Beijing Sanju Environmental Protection and New Material Co., Ltd. | Composition of amorphous iron oxide hydroxide, desulfurizer comprising the same, and methods for preparing and regenerating the desulfurizer |
| US7717979B2 (en) | 2006-08-28 | 2010-05-18 | Beijing Sj Environmental Protection And New Material Co., Ltd. | Composition for a desulfurizer with a high sulfur capacity and the process of making the same |
| CN101584962B (en) * | 2008-05-23 | 2012-07-18 | 北京三聚环保新材料股份有限公司 | High-strength FeOOH desulfurizer and preparation method thereof |
| CN101590396B (en) * | 2008-05-30 | 2012-02-15 | 北京三聚环保新材料股份有限公司 | Method for preparing and producing high-sulphur capacity iron-based desulfurizer |
| CN101711925A (en) * | 2008-10-02 | 2010-05-26 | 巴斯夫欧洲公司 | Method for depletion of sulfur and/or compounds containing sulfur from a biochemically produced organic compound |
| CN101711925B (en) * | 2008-10-02 | 2014-12-10 | 巴斯夫欧洲公司 | Method for depletion of sulfur and/or compounds containing sulfur from a biochemically produced organic compound |
| US8647600B2 (en) | 2008-12-30 | 2014-02-11 | Beijing Sanju Environmental Protection and New Material Co., Ltd. | Methods for preparing and regenerating materials containing amorphous iron oxide hydroxide and desulfurizer comprising the same |
| US8591847B2 (en) | 2008-12-30 | 2013-11-26 | Beijing Sanju Environmental Protection and New Material Co., Ltd. | Method for removing hydrogen sulfide from gaseous stream at normal temperature |
| US8585993B2 (en) | 2008-12-30 | 2013-11-19 | Beijing Sanju Enviromental Protection and New Material Co., Ltd. | Method for regenerating amorphous iron oxide hydroxide and desulfurizer containing amorphous iron oxide hydroxide as active component |
| US8652427B2 (en) | 2008-12-30 | 2014-02-18 | Beijing Sanju Environmental Protection and New Material Co., Ltd. | Preparation and repeated regeneration of material containing amorphous iron oxide hydroxide, desulfurization agents containing the material, and preparation and repeated regeneration thereof |
| US9283539B2 (en) | 2008-12-30 | 2016-03-15 | Beijing Sanju Environmental Protection and New Material Co., Ltd. | Methods for preparing and regenerating materials containing amorphous iron oxide hydroxide and desulfurizer comprising the same |
| CN101798625A (en) * | 2010-04-14 | 2010-08-11 | 北京科技大学 | Method for removing sulfur from fuel before sintering iron ores |
| CN104645951A (en) * | 2013-11-21 | 2015-05-27 | 东营科尔特化工科技有限公司 | Regeneration method of fine desulfuration agent of liquefied petroleum gas |
| CN105771620A (en) * | 2016-05-05 | 2016-07-20 | 张锐 | Efficient desulfurizer and preparation method thereof |
| CN106139880A (en) * | 2016-06-28 | 2016-11-23 | 安徽国能亿盛环保科技有限公司 | A kind of industrial waste gas desulfurizing agent and preparation method thereof |
| CN110564457A (en) * | 2019-07-26 | 2019-12-13 | 沈阳三聚凯特催化剂有限公司 | Deep purification fine desulfurizer and preparation method thereof |
| CN115093005A (en) * | 2022-06-27 | 2022-09-23 | 中节能工程技术研究院有限公司 | Waste alkali liquor oxidation desulfurization method |
| CN115093005B (en) * | 2022-06-27 | 2023-11-10 | 中节能工程技术研究院有限公司 | Waste alkali liquid oxidation desulfurization method |
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