CN104437072B - A kind of preparation method of middle desulfurizing agent for high-temp gas - Google Patents
A kind of preparation method of middle desulfurizing agent for high-temp gas Download PDFInfo
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Abstract
The invention provides a kind of preparation method of middle desulfurizing agent for high-temp gas, for desulfurizing agent presoma zinc sulphide is prepared in raw material solid phase reaction with zinc acetate and vulcanized sodium, again that zinc sulphide and binding agent kaolin, pore creating material starch ground is kneaded and formed, first roasting in a nitrogen atmosphere, pass into oxygen-containing atmosphere at same temperature, in-situ regeneration method obtains fresh desulfurizing agent zinc oxide.Desulfurizing agent prepared by the present invention has two-stage pore structure, and pore structure is abundant, desulfurization performance is excellent, after repeatedly sulfuration regeneration cycle, still can keep good desulfurization performance.
Description
Technical field
The present invention relates to a kind of preparation method of gas desulfurizer, particularly relate to a kind of preparation method of middle high-temperature dry coal gas desulfurization desulfurizing agent.
Background technology
The few oil of the rich coal lean gas of China, consumption of coal accounts for about 70% of total energy consumption figure, and the energy resource structure based on coal cannot change within short-term.Coal Gasification is the leading technology of Coal Chemical Industry, and the clean and effective that can realize coal utilizes.The raw gas that gasification furnace produces contains H
2the toxic gases such as S, and H
2s can poison catalyst, etching apparatus and pipeline, and sulfurous gas sucks serious harm health, therefore H after human body
2removing of S seems particularly necessary.
Coal gas desulfurization technology comprises wet desulphurization and dry desulfurization two kinds of methods.Wet Flue Gas Desulfurization Technique treating capacity is large, technology relative maturity, but this technology exists the shortcomings such as gas heat utilization ratio is low, water consumption is large, desulfuration efficiency is low.Middle high-temperature dry coal gas desulfurization can significantly improve the utilization rate of gas heat, and has the high advantage of desulfuration efficiency, is applicable to H
2the essence of S removes.
Middle desulfurizing agent for high-temp gas is mainly based on single metal oxides and composite metal oxide, its preparation method is generally the presoma first being prepared desulphurizing activated component by methods such as solid phase method, infusion process, the precipitation method, and then obtain desulphurizing activated component through roasting, finally mix with binding agent, pore creating material, make desulfurizing agent through high-temperature roasting.
CN1317548A, CN103184079A, CN101440313A all disclose the preparation method of desulfurizing agent, its common ground is: after the shaping oven dry of desulfurizing agent, obtain the fresh desulfurizing agent with certain pore structure through an one-step baking, namely just secured the pore structure of desulfurizing agent by high-temperature process.Obviously, desulfurizing agent prepared by above-mentioned conventional method only has one-level pore structure, and one-level pore structure is easily destroyed in sulfuration regeneration cycle, makes desulfurizing agent after repeatedly sulfuration regeneration cycle, occurs that Sulfur capacity declines obvious phenomenon.
Summary of the invention
The object of this invention is to provide a kind of preparation method of novel middle desulfurizing agent for high-temp gas, to make desulfurizing agent still can keep good pore structure after repeatedly sulfuration regeneration cycle, there will not be the phenomenon that Sulfur capacity obviously reduces.
The invention provides a kind of method adopting desulfurizing agent for high-temp gas in situ regeneration method preparation, concrete grammar is:
1) zinc acetate and vulcanized sodium are ground according to the mixed in molar ratio of 1 ︰ (1 ~ 2) carry out solid phase reaction, after washing away impurity sodium acetate, obtain desulfurizing agent presoma zinc sulphide;
2) by 20 ~ 45wt% zinc sulphide, 40 ~ 70wt% binding agent kaolin, the mixing of 5 ~ 10wt% pore creating material starch, be ground to below 200 orders, add water kneading, extrusion, drying forming;
3) shaping rear material 500 ~ 650 DEG C of roasting 1 ~ 2h in a nitrogen atmosphere, pass into oxygen-containing atmosphere at same temperature, in-situ regeneration method obtains fresh desulfurizing agent zinc oxide.
Wherein, described oxygen-containing atmosphere is the mist of air and nitrogen or the mist of oxygen and nitrogen, and in mist, the content of oxygen is 5 ~ 10%.
Further, passing into the time that oxygen-containing atmosphere carries out oxidation processes is 1 ~ 3h.
In the present invention, preferably zinc acetate and vulcanized sodium are ground 1 ~ 4h with the speed of 300 ~ 500r/min in ball mill.
According to theory analysis, when metal sulfide regenerates under an oxygen-containing atmosphere, its sulphur atom is displaced by oxygen atom, and the atomic radius of the latter is less than the former, so can produce some pore structures in this process.The present invention, first by metal sulfide and auxiliary agent, pore creating material mixed-forming, generates one-level pore structure by drying roasting; While roasting, by oxygen-containing atmosphere process, metal sulfide is made to become metal oxide (being similar to regenerative response), this process meeting regeneration part pore structure (second hole gap structure), therefore, the desulfurizing agent that prepared by the inventive method can possess two-stage pore structure.
Analyze from principle, desulfurizing agent prepared by above-mentioned employing two step high-temperature process, its one-level pore structure remains unchanged in sulfuration regeneration cycle, the just second hole gap structure changed, this just can make desulfurizing agent after sulfuration regeneration cycle repeatedly, still can keep good pore structure, after repeatedly sulfuration regeneration cycle, there will not be the phenomenon that Sulfur capacity obviously reduces.
Desulfurizing agent prepared by the present invention is mainly used in middle high temperature coal gas purification field as dry method H
2s desulfurizing agent, desulfurization temperature is 450 ~ 600 DEG C.
The fresh sample pore structure of the desulfurizing agent prepared in the process of the present invention is good, and desulfurization performance is excellent, and Sulfur capacity is 90 ~ 95% of theoretical Sulfur capacity; Simultaneously desulfurizing agent still has good pore structure after repeatedly sulfuration, and still can keep good Sulfur capacity after ten sulfuration regeneration cycle, its Sulfur capacity value is more than 85% of a Sulfur capacity; Meanwhile, the desulfurizing agent that prepared by the inventive method (1 ~ 3h) can complete regeneration in the short period of time.
Detailed description of the invention
Embodiment 1
Take zinc acetate 45g, vulcanized sodium 22g, after mixing, put into ball mill, with the rotating speed of 300r/min grinding 1h.Impurity sodium acetate is washed away, can't detect acetate ion in filtrate till by deionized water.
Take obtained zinc sulphide 20g, mix with 70g kaolin, 10g starch, put into ball mill, be ground to below 200 orders with the rotating speed of 400r/min, add deionized water kneading, extruded moulding.
Shaping rear sample dries 1h at 85 DEG C in baking oven, makes the bar shaped desulfurizing agent of diameter 3mm, long 3mm; And be placed in tube furnace (bore 5cm), at 500 DEG C, roasting 1h under the nitrogen atmosphere of flow velocity 200mL/min; Switched to by gas air and nitrogen volume ratio to be the mist of 1 ︰ 3, at 500 DEG C, under the oxygen-containing atmosphere of flow velocity 500mL/min, continue roasting 2h, obtain Zinc oxide desulfurizer finished product A1(zinc oxide content 19%).
Take zinc hydroxide 20.1g, after mixing with 70g kaolin, 10g starch, put into ball mill, be ground to below 200 orders with the rotating speed of 400r/min, add deionized water kneading, extruded moulding; Shaping rear sample dries 1h at 85 DEG C in baking oven, makes the bar shaped desulfurizing agent of diameter 3mm, long 3mm, and 500 DEG C of calcining 3h, namely obtain desulfurizing agent finished product B1, wherein zinc oxide content is also 19%.
HDS evaluation condition: reaction atmosphere simulation texaco gasification coal gas (39%H
2, 0.2 ~ 0.3%H
2s, 27%CO, 12%CO
2, 10%H
2o, N
2for Balance Air).Doctor solution consumption 15g, desulfurization temperature 450 DEG C, air speed 2000h
-1.Desulfurizer regeneration condition: regeneration atmosphere 4%O
2+ 96%N
2, air speed 3000h
-1, regeneration temperature 500 DEG C.
Desulfurized effect compares in table 1.
Embodiment 2
Take zinc acetate 69g, vulcanized sodium 36g, after mixing, put into ball mill, with the rotating speed of 400r/min grinding 2h.Impurity sodium acetate is washed away, can't detect acetate ion in filtrate till by deionized water.
Take obtained zinc sulphide 20g, mix with 42g kaolin, 4.7g starch, put into ball mill, be ground to below 200 orders with the rotating speed of 400r/min, add deionized water kneading, extruded moulding.
Shaping rear sample dries 1h at 85 DEG C in baking oven, makes the bar shaped desulfurizing agent of diameter 3mm, long 3mm; And be placed in tube furnace (bore 5cm), at 550 DEG C, roasting 1h under the nitrogen atmosphere of flow velocity 200mL/min; Switched to by gas air and nitrogen volume ratio to be the mist of 1 ︰ 1.5, at 550 DEG C, under the oxygen-containing atmosphere of flow velocity 500mL/min, continue roasting 1.5h, obtain Zinc oxide desulfurizer finished product A2(zinc oxide content 28%).
Take zinc hydroxide 20g, after mixing with 42g kaolin, 4.7g starch, put into ball mill, be ground to below 200 orders with the rotating speed of 400r/min, add deionized water kneading, extruded moulding; Shaping rear sample dries 1h at 85 DEG C in baking oven, makes the bar shaped desulfurizing agent of diameter 3mm, long 3mm, and 550 DEG C of calcining 2.5h, namely obtain desulfurizing agent finished product B2, wherein zinc oxide content is also 28%.
HDS evaluation condition: reaction atmosphere simulation texaco gasification coal gas, doctor solution consumption 15g, desulfurization temperature 500 DEG C, air speed 2000h
-1.Desulfurizer regeneration condition: regeneration atmosphere 5%O
2+ 95%N
2, air speed 3000h
-1, regeneration temperature 500 DEG C.
Desulfurized effect compares in table 1.
Embodiment 3
Take zinc acetate 69g, vulcanized sodium 36g, after mixing, put into ball mill, with the rotating speed of 400r/min grinding 3h.Impurity sodium acetate is washed away, can't detect acetate ion in filtrate till by deionized water.
Take obtained zinc sulphide 25g, mix with 20g kaolin, 5g starch, put into ball mill, be ground to below 200 orders with the rotating speed of 400r/min, add deionized water kneading, extruded moulding.
Shaping rear sample dries 1h at 85 DEG C in baking oven, makes the bar shaped desulfurizing agent of diameter 3mm, long 3mm; And be placed in tube furnace (bore 5cm), at 650 DEG C, roasting 1h under the nitrogen atmosphere of flow velocity 200mL/min; Switched to by gas air and nitrogen volume ratio to be the mist of 1 ︰ 1, at 650 DEG C, under the oxygen-containing atmosphere of flow velocity 500mL/min, continue roasting 1h, obtain Zinc oxide desulfurizer finished product A3(zinc oxide content 51%).
Take zinc hydroxide 25.4g, after mixing with 20g kaolin, 5g starch, put into ball mill, be ground to below 200 orders with the rotating speed of 400r/min, add deionized water kneading, extruded moulding; Shaping rear sample dries 1h at 85 DEG C in baking oven, makes the bar shaped desulfurizing agent of diameter 3mm, long 3mm, and 650 DEG C of calcining 2h, namely obtain desulfurizing agent finished product B3, wherein zinc oxide content is also 51%.
HDS evaluation condition: reaction atmosphere simulation texaco gasification coal gas, doctor solution consumption 15g, desulfurization temperature 450 DEG C, air speed 2000h
-1.Desulfurizer regeneration condition: regeneration atmosphere 8%O
2+ 92%N
2, air speed 3000h
-1, regeneration temperature 500 DEG C.
Desulfurized effect compares in table 1.
Embodiment 4
Take zinc acetate 45.9g, vulcanized sodium 23.4g, after mixing, put into ball mill, with the rotating speed of 500r/min grinding 4h.Impurity sodium acetate is washed away, can't detect acetate ion in filtrate till by deionized water.
Take obtained zinc sulphide 22.2g, mix with 20g kaolin, 2.2g starch, put into ball mill, be ground to below 200 orders with the rotating speed of 400r/min, add deionized water kneading, extruded moulding.
Shaping rear sample dries 1h at 85 DEG C in baking oven, makes the bar shaped desulfurizing agent of diameter 3mm, long 3mm; And be placed in tube furnace (bore 5cm), at 500 DEG C, roasting 2h under the nitrogen atmosphere of flow velocity 200mL/min; Switched to by gas air and nitrogen volume ratio to be the mist of 1 ︰ 3, at 500 DEG C, under the oxygen-containing atmosphere of flow velocity 500mL/min, continue roasting 2.5h, obtain Zinc oxide desulfurizer finished product A4(zinc oxide content 48%).
Take zinc hydroxide 22.6g, after mixing with 20g kaolin, 2.2g starch, put into ball mill, be ground to below 200 orders with the rotating speed of 400r/min, add deionized water kneading, extruded moulding; Shaping rear sample dries 1h at 85 DEG C in baking oven, makes the bar shaped desulfurizing agent of diameter 3mm, long 3mm, and 500 DEG C of calcining 4.5h, namely obtain desulfurizing agent finished product B4, wherein zinc oxide content is also 48%.
HDS evaluation condition: reaction atmosphere simulation texaco gasification coal gas, doctor solution consumption 15g, desulfurization temperature 600 DEG C, air speed 2000h
-1.Desulfurizer regeneration condition: regeneration atmosphere 8%O
2+ 92%N
2, air speed 3000h
-1, regeneration temperature 500 DEG C.
Desulfurized effect compares in table 1.
Embodiment 5
Take zinc acetate 45g, vulcanized sodium 22g, after mixing, put into ball mill, with the rotating speed of 400r/min grinding 2h.Impurity sodium acetate is washed away, can't detect acetate ion in filtrate till by deionized water.
Take obtained zinc sulphide 20g, mix with 70g kaolin, 10g starch, put into ball mill, be ground to below 200 orders with the rotating speed of 400r/min, add deionized water kneading, extruded moulding.
Shaping rear sample dries 1h at 85 DEG C in baking oven, makes the bar shaped desulfurizing agent of diameter 3mm, long 3mm; And be placed in tube furnace (bore 5cm), at 500 DEG C, roasting 1h under the nitrogen atmosphere of flow velocity 200mL/min; Switched to by gas oxygen and nitrogen volume ratio to be the mist of 1 ︰ 9, at 500 DEG C, under the oxygen-containing atmosphere of flow velocity 500mL/min, continue roasting 2h, obtain Zinc oxide desulfurizer finished product A5(zinc oxide content 19%).
Take zinc acetate 37.2g, oxalic acid 18.2g, after mixing with 70g kaolin, 10g starch, put into ball mill, be ground to below 200 orders with the rotating speed of 400r/min, add deionized water kneading, extruded moulding; Shaping rear sample dries 1h at 85 DEG C in baking oven, makes the bar shaped desulfurizing agent of diameter 3mm, long 3mm, and 500 DEG C of calcining 3h, namely obtain desulfurizing agent finished product B5, wherein zinc oxide content is also 19%.
HDS evaluation condition: reaction atmosphere simulation texaco gasification coal gas, doctor solution consumption 15g, desulfurization temperature 450 DEG C, air speed 2000h
-1.Desulfurizer regeneration condition: regeneration atmosphere 6%O
2+ 94%N
2, air speed 3000h
-1, regeneration temperature 500 DEG C.
Desulfurized effect compares in table 1.
Embodiment 6
Take zinc acetate 69g, vulcanized sodium 36g, after mixing, put into ball mill, with the rotating speed of 400r/min grinding 2h.Impurity sodium acetate is washed away, can't detect acetate ion in filtrate till by deionized water.
Take obtained zinc sulphide 20g, mix with 42g kaolin, 4.7g starch, put into ball mill, be ground to below 200 orders with the rotating speed of 400r/min, add deionized water kneading, extruded moulding.
Shaping rear sample dries 1h at 85 DEG C in baking oven, makes the bar shaped desulfurizing agent of diameter 3mm, long 3mm; And be placed in tube furnace (bore 5cm), at 500 DEG C, roasting 1h under the nitrogen atmosphere of flow velocity 200mL/min; Switched to by gas air and nitrogen volume ratio to be the mist of 1 ︰ 1.5, at 500 DEG C, under the oxygen-containing atmosphere of flow velocity 500mL/min, continue roasting 2h, obtain Zinc oxide desulfurizer finished product A6(zinc oxide content 28%).
Take zinc acetate 37g, oxalic acid 18.1g, after mixing with 42g kaolin, 4.7g starch, put into ball mill, be ground to below 200 orders with the rotating speed of 400r/min, add deionized water kneading, extruded moulding; Shaping rear sample dries 1h at 85 DEG C in baking oven, makes the bar shaped desulfurizing agent of diameter 3mm, long 3mm, and 500 DEG C of calcining 3h, namely obtain desulfurizing agent finished product B6, wherein zinc oxide content is also 28%.
HDS evaluation condition: reaction atmosphere simulation texaco gasification coal gas, doctor solution consumption 15g, desulfurization temperature 450 DEG C, air speed 2000h
-1.Desulfurizer regeneration condition: regeneration atmosphere 8%O
2+ 92%N
2, air speed 3000h
-1, regeneration temperature 500 DEG C.
Desulfurized effect compares in table 1.
Claims (5)
1. a preparation method for desulfurizing agent for high-temp gas in, comprises the following steps:
1) zinc acetate and vulcanized sodium are ground according to the mixed in molar ratio of 1 ︰ (1 ~ 2) carry out solid phase reaction, after washing away impurity sodium acetate, obtain desulfurizing agent presoma zinc sulphide;
2) by 20 ~ 45wt% zinc sulphide, 40 ~ 70wt% binding agent kaolin, the mixing of 5 ~ 10wt% pore creating material starch, be ground to below 200 orders, add water kneading, extrusion, drying forming;
3) shaping rear material 500 ~ 650 DEG C of roasting 1 ~ 2h in a nitrogen atmosphere, pass into oxygen-containing atmosphere at same temperature, in-situ regeneration method obtains fresh desulfurizing agent zinc oxide.
2. the preparation method of middle desulfurizing agent for high-temp gas according to claim 1, is characterized in that described oxygen-containing atmosphere is the mist of air and nitrogen or the mist of oxygen and nitrogen.
3. the preparation method of middle desulfurizing agent for high-temp gas according to claim 1, is characterized in that the oxygen content in described mist is 5 ~ 10%.
4. the preparation method of middle desulfurizing agent for high-temp gas according to claim 1, it is characterized in that passing into the time that oxygen-containing atmosphere carries out oxidation processes is 1 ~ 3h.
5. the preparation method of middle desulfurizing agent for high-temp gas according to claim 1, is characterized in that zinc acetate and vulcanized sodium to grind 1 ~ 4h with the speed of 300 ~ 500r/min in ball mill.
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| CN106336910A (en) * | 2016-10-21 | 2017-01-18 | 太原理工大学 | Method for utilizing microwave in-situ synthesis to prepare zinc-ferrite desulfurizing agent |
| CN106497613B (en) * | 2016-10-21 | 2019-09-27 | 太原理工大学 | A kind of method that microwave prepares iron oxide high temperature gas desulfurizer |
| CN108905959B (en) * | 2018-07-09 | 2021-02-23 | 太原理工大学 | Method for preparing ZnO/MCM-41 desulfurizer by microwave in-situ one-step method |
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| JP2007002061A (en) * | 2005-06-22 | 2007-01-11 | Mitsubishi Heavy Ind Ltd | Gas cleaning apparatus, gasification system, gasification power generation system |
| CN101590360B (en) * | 2008-05-29 | 2013-04-17 | 北京三聚环保新材料股份有限公司 | Improved high temperature desulfuration agent and preparation method thereof |
| CN101735861B (en) * | 2009-12-11 | 2012-12-19 | 太原理工大学 | Zinc oxide medium and high temperature coal gas fine desulfurizer and preparation method |
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