CN102049257A - Catalyst for simultaneously reducing SO2 and NO with CO as well as preparation and application of catalyst - Google Patents

Catalyst for simultaneously reducing SO2 and NO with CO as well as preparation and application of catalyst Download PDF

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CN102049257A
CN102049257A CN2009101881570A CN200910188157A CN102049257A CN 102049257 A CN102049257 A CN 102049257A CN 2009101881570 A CN2009101881570 A CN 2009101881570A CN 200910188157 A CN200910188157 A CN 200910188157A CN 102049257 A CN102049257 A CN 102049257A
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catalyst
tio
carrier
transition metal
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CN102049257B (en
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王学海
方向晨
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中国石油化工股份有限公司
中国石油化工股份有限公司抚顺石油化工研究院
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    • Y02A50/2344
    • Y02A50/2349

Abstract

The invention discloses a catalyst for simultaneously reducing SO2 and NO with CO as well as a preparation method of the catalyst. In the catalyst, a TiO2-Al2O3 compound is used as a carrier, wherein the weight of TiO2 accounts for 5-20% of the weight of the carrier; and an active component is one or more of transition metal oxides, and the load amount of the active component is 5-30% based on an oxide by weight. The catalyst is prepared by the following steps: firstly, adopting an immersion method to load TiO2 on Al2O3; and then introducing active component through a precursor solution used for immersing the active component. The catalyst has high activity in the reaction that SO2 and NO are reduced by CO at the same time; and under the lower reaction temperature and high airspeed, the conversion rate of SO2 can reach 98%, and the conversion rate of NO is nearly 100%.

Description

CO reduces SO simultaneously 2Catalyst and preparation and application with NO

Technical field

The present invention relates to a kind of SO that reduces simultaneously 2With the Catalysts and its preparation method of NO, relate in particular to a kind of CO and reduce SO simultaneously 2Catalysts and its preparation method and application with NO.

Background technology

Sulfur dioxide (SO 2) and nitrogen oxide (NOx) be the major pollutants of atmosphere, they can produce acid rain, form photochemical fog, destroy ozone, bring great harm for environment and human health.China is to be the country of main energy sources with the coal, and the SO in the flue gas discharges in the coal-burning power plant 2Account for 90% of total amount with NOx, all the other come from discharged flue gas in the industrial production such as petroleum refining.At present, the annual SO of China 2Discharge capacity surpassed 2,500 ten thousand tons, become SO in the world 2The first discharging big country; The discharge capacity in NOx every year has also surpassed 1,000 ten thousand tons.Desulphurization denitration is the key subjects of China's air contaminant treatment.

Using at present flue gas desulfurization and denitration technique more widely in the world and be traditional desulfur technology (FGD) the combined selective catalytic reduction technology (SCR) of application works alone separately and removes SO in the flue gas respectively 2Combined desulfurization and denitration technology with NOx.For example: lime/lime stone-SCR technology and SNOX TMTechnology.The combined desulfurization and denitration technology generally all has comparatively ideal denitrification efficiency, but owing to adopt two covering devices to carry out desulfurization and denitration respectively, has therefore that floor space is big, flow process is complicated, investment and shortcomings such as operating cost height, secondary pollution.

Therefore usually contain CO in the flue gas, utilize CO in the flue gas to reduce SO simultaneously 2With NO be elemental sulfur and N 2Not only can eliminate these three kinds of pollutants simultaneously, and this technical process is simple, no waste liquid and waste residue, the catalyst with high activity, selectivity and stability is the core place of this technology.

US 5853684 discloses a kind of CO and has reduced SO simultaneously 2With the catalyst of NO, this catalyst is the oxysulfide of transition metal and rare earth metal, as CoS 2-La 2O 2S.This catalyst desired reaction temperature height, at 500 ℃, SO 2Conversion ratio be 98%, the NO conversion ratio is 100%.

CN 1288773A discloses a kind of CO and has reduced SO simultaneously 2With the catalyst of NO, this catalyst is the tin ash of coprecipitation preparation and the composite oxides of titanium dioxide.The disclosed catalyst of CN 1288774A is carrier with titanium dioxide, and active component is the oxide of cobalt and nickel, and the auxiliary activity component is molybdenum, tungsten and rare earth metal.More than two kinds of catalyst all can get 98% SO at 350 ℃ 2Conversion ratio and 100% NO conversion ratio, but reaction velocity is low, has only 8000h -1

At present, relevant both at home and abroad CO reduces SO simultaneously 2Less with the patent of NO catalyst, there is the high and low shortcoming of air speed of reaction temperature in the catalyst of existing publication.

Summary of the invention

At the deficiencies in the prior art, the invention provides a kind of CO and reduce SO simultaneously 2With the catalyst of NO, this catalyst reduces SO simultaneously to CO 2Reaction has very high activity with NO, under lower reaction temperature and high-speed, can get 98% SO 2Conversion ratio and the NO conversion ratio that is close to 100%.

The invention provides a kind of CO and reduce SO simultaneously 2With the catalyst of NO, described catalyst comprises:

(1) carrier: with TiO 2-Al 2O 3Compound is a carrier, TiO 2Spread loads is in Al 2O 3Surface, wherein TiO 2Weight content in carrier is 5%~25%, is preferably 5%~20%;

(2) active component: the activity of such catalysts component is one or more in the transition metal oxide, and the content of active component counts 1%~35% with oxide, is preferably 5%~30%.

Wherein said Al 2O 3Be γ-Al 2O 3

Wherein said transition metal is selected from one or more among Fe, Co, Ni, Cu, Mo and the W.

According to a second aspect of the invention, also provide the preparation method of above-mentioned reducing catalyst, said method comprising the steps of:

(1) at first with Al 2O 3Impregnated in TiO 2Precursor solution in, obtain TiO after drying and the roasting 2-Al 2O 3Complex carrier;

(2) TiO that step (1) is prepared 2-Al 2O 3Complex carrier impregnated in the salting liquid of transition metal, and drying and roasting obtain the catalyst of carrying transition metal oxide.

According to method provided by the invention, the TiO described in the step (1) 2Precursor solution is selected from one group of material that ethanolic solution, titanium sulfate aqueous solution or the aqueous solution of titanyle sulfate of ethanolic solution, the titanium tetrachloride of butyl titanate are formed.

100~120 ℃ of baking temperatures described in step (1) and the step (2), 6~12 hours drying times; Described sintering temperature 400-600 ℃, roasting time 2~5 hours.

Transition metal described in the step (2) is selected from one or more among Fe, Co, Ni, Cu, Mo, the W.The salting liquid of described transition metal generally includes: the nitrate of Fe, Co, Ni, Cu, sulfate; Ammonium molybdate; Ammonium tungstate.

According to a third aspect of the present invention, the present invention also provides a kind of described catalyst to reduce SO simultaneously at CO 2With the application among the NO: above-mentioned catalytic reduction catalysts is placed reactor, feeds CO, SO 2The reaction gas of forming with NO reacts, and wherein reaction temperature is 320~350 ℃, and reaction velocity is 5000h -1~20000h -1

According to the conventional method in this area, described catalyst can carry out presulfurization under 400~600 ℃ in the presence of sulfurous gas before using.This presulfurization can be carried out also can original position vulcanizing in device outside device, is translated into sulphided state.

Described sulfurous gas is H 2S, SO 2/ CO or SO 2/ H 2

Compared with prior art, the present invention has following characteristics:

1, catalyst of the present invention is with TiO 2The Al of modification 2O 3Be carrier, through TiO 2After the modification, the pore volume of complex carrier and specific area also further increase.After reactive metal loads to this complex carrier, disperse more evenly, thereby the more existing reducing catalyst of activity of such catalysts is significantly improved.And Preparation of catalysts method of the present invention is simple, and flow process is simple.

2, sulfur dioxide and nitrogen oxide during reducing catalyst of the present invention can remove smoke simultaneously can be simplified the process for purifying of purifying contaminated gas significantly.Reducing catalyst of the present invention is used for CO and reduces SO simultaneously 2When reacting, shown high reactivity with NO.Catalyst of the present invention is (20000h under lower temperature (320 ℃) and high-speed -1) can obtain 98% SO 2Conversion ratio and the NO conversion ratio that is close to 100%.

The specific embodiment

The specific embodiment of the present invention will be described in more detail technical scheme of the present invention by following examples, and described embodiment should not be construed as the restriction of the scope of the invention.

Embodiment 1

With Al 2O 3Impregnated in the ethanolic solution of an amount of butyl titanate, stir evaporate to dryness, left standstill 12 hours, through 100 ℃ of dryings 12 hours, 500 ℃ of roastings obtained TiO after 4 hours 2-Al 2O 3Complex carrier;

With TiO 2-Al 2O 3Complex carrier impregnated in the iron nitrate aqueous solution, stirs evaporate to dryness, and through 110 ℃ of dryings 12 hours, 600 ℃ of roastings obtained the catalyst of load iron oxide in 2 hours, were numbered C 1

Above-mentioned catalyst under 400 ℃, is fed H 2S gas cure 5 hours.

In the gained catalyst, TiO 2Account for 5% of vehicle weight; The iron oxide load capacity is 5%.

Embodiment 2

With Al 2O 3Impregnated in the ethanolic solution of an amount of titanium tetrachloride, stir evaporate to dryness, left standstill 12 hours, through 110 ℃ of dryings 8 hours, 600 ℃ of roastings obtained TiO after 2 hours 2-Al 2O 3Complex carrier;

With TiO 2-Al 2O 3Complex carrier impregnated in an amount of cobalt nitrate aqueous solution, stirs evaporate to dryness, and through 100 ℃ of dryings 12 hours, 500 ℃ of roastings obtained the catalyst of load cobalt oxide in 3 hours, were numbered C 2

Above-mentioned catalyst under 500 ℃, is fed H 2S gas cure 3 hours.

In the gained catalyst, TiO 2Account for 15% of vehicle weight; The supported by cobalt oxide amount is 10%

Embodiment 3

With Al 2O 3Impregnated in the aqueous solution of an amount of titanium sulfate, stir evaporate to dryness, left standstill 12 hours, through 120 ℃ of dryings 6 hours, 400 ℃ of roastings obtained TiO after 5 hours 2-Al 2O 3Complex carrier;

With TiO 2-Al 2O 3Complex carrier impregnated in an amount of cobalt nitrate and the ammonium molybdate mixed aqueous solution, stirs evaporate to dryness, and through 120 ℃ of dryings 6 hours, 400 ℃ of roastings obtained the catalyst of load cobalt oxide and molybdenum oxide in 5 hours, were numbered C 3

Above-mentioned catalyst under 500 ℃, is fed SO 2/ CO gas cure 5 hours.

In the gained catalyst, TiO 2Account for 10% of vehicle weight; The supported by cobalt oxide amount is 10%, the molybdenum oxide load capacity is 10%.

Embodiment 4

With Al 2O 3Impregnated in the aqueous solution of an amount of titanyl sulfate, stir evaporate to dryness, left standstill 12 hours, through 100 ℃ of dryings 12 hours, 500 ℃ of roastings obtained TiO after 5 hours 2-Al 2O 3Complex carrier;

With TiO 2-Al 2O 3Complex carrier impregnated in an amount of nickel nitrate aqueous solution, stirs evaporate to dryness, and through 120 ℃ of dryings 6 hours, 600 ℃ of roastings obtained the catalyst of load nickel oxide in 3 hours, were numbered C 4

Above-mentioned catalyst under 600 ℃, is fed SO 2/ H 2Gas cure 3 hours.

In the gained catalyst, TiO 2Account for 20% of vehicle weight; Nickel oxide loaded amount is 30%.

Embodiment 5

With Al 2O 3Impregnated in the aqueous solution of an amount of titanium sulfate, stir evaporate to dryness, left standstill 12 hours, obtain TiO after drying and the roasting 2-Al 2O 3Complex carrier;

With TiO 2-Al 2O 3Complex carrier impregnated in an amount of ferric nitrate and nickel nitrate aqueous solution, stirs evaporate to dryness, and drying and roasting obtain the catalyst of load nickel oxide, are numbered C 5

Above-mentioned catalyst under 400 ℃, is fed SO 2/ H 2Gas cure 3 hours.

In the gained catalyst, TiO 2Account for 20% of vehicle weight; The iron oxide load capacity is 10%, nickel oxide loaded amount is 10%.

Comparative example 1

According to CN1288774A embodiment 1 preparation catalyst C 6, catalyst consists of: MoO 3/ TiO 2-Co 3O 4, wherein, the weight ratio of titanium dioxide and cobalt oxide is 1: 1, MoO 3Account for 15% of catalyst total amount.

Comparative example 2

According to CN 1288773A embodiment 1 preparation catalyst C 7, catalyst consists of: SnO 2-TiO 2, the weight ratio of tin ash and titanium dioxide is 1: 1..

Comparative example 3

Prepare catalyst C according to embodiment among the US 5853684 8, catalyst consists of: CoS 2-La 2O 2S, the mass ratio of Co and La 2.3: 1.

Embodiment 6

The catalyst of embodiment 1-5 and comparative example 1-3 preparation reduces SO simultaneously at CO 2With the application among the NO.Application test carries out on the small-sized evaluating apparatus in laboratory.The concentration of reaction gas is: SO 21200 μ L/L, NO 1000 μ L/L and CO 3400 μ L/L; Air speed: 20000h -1The elemental sulfur that reaction end gas generates by the cooling of frozen water cold-trap earlier is then through gas-chromatography HP-6890 on-line analysis, the SO in the tail gas 2, CS 2Separated by Gaspro Capillary capillary column with COS, FPD detects; CO and CO 2Separated by Porapack Q packed column, TCD detects.N 2Separate with the 5A molecular sieve, TCD detects.SO 2Conversion ratio (X SO2), the selectivity (Y of elemental sulfur s), the yield (Y) and the NO conversion ratio (X of elemental sulfur NO) calculate by following formula: result of the test is listed in the table 1.

X SO 2 [ SO 2 ] in - [ SO 2 ] out [ SO 2 ] in * 100 %

Y s = [ SO 2 ] in - [ SO 2 ] out - [ COS ] out - [ CS 2 ] out [ SO 2 ] in - [ SO 2 ] out * 100 %

Y=XY s

X NO = 2 [ N 2 ] out [ NO ] in * 100 %

Table 1

By the contrast experiment as can be known, catalyst of the present invention reduces SO than the catalyst of existing patent report simultaneously to CO 2Reaction has better low temperature active with NO.

Claims (9)

1. a CO reduces SO simultaneously 2With the catalyst of NO, described catalyst comprises:
(1) carrier: with TiO 2-Al 2O 3Compound is a carrier, TiO 2Spread loads is in Al 2O 3Surface, wherein TiO 2Weight content in carrier is 5%~25%;
(2) active component: the activity of such catalysts component is one or more in the transition metal oxide, and the content of active component counts 1%~35% with oxide.
2. according to the described catalyst of claim 1, it is characterized in that described TiO 2Weight content in carrier is 5%~20%, and the content of described active component in catalyst counts 5%~30% with oxide.
3. according to the described catalyst of claim 1, it is characterized in that described transition metal is selected from one or more among Fe, Co, Ni, Cu, Mo and the W.
4. the described Preparation of catalysts method of the arbitrary claim of claim 1~3 may further comprise the steps:
(1) at first with Al 2O 3Impregnated in TiO 2Precursor solution in, obtain TiO after drying and the roasting 2-Al 2O 3Complex carrier;
(2) TiO that step (1) is prepared 2-Al 2O 3Complex carrier impregnated in the salting liquid of transition metal, and drying and roasting obtain the catalyst of carrying transition metal oxide.
5. according to the described preparation method of claim 4, it is characterized in that the TiO described in the step (1) 2Precursor solution is selected from one group of material that ethanolic solution, titanium sulfate aqueous solution or the aqueous solution of titanyle sulfate of ethanolic solution, the titanium tetrachloride of butyl titanate are formed.
6. according to the described preparation method of claim 4, it is characterized in that the baking temperature described in step (1) and the step (2) is 100~120 ℃, be 6~12 hours drying time; Described sintering temperature is 400~600 ℃, and roasting time is 2~5 hours.
7. according to the described preparation method of claim 4, it is characterized in that the transition metal described in the step (2) is selected from one or more among Fe, Co, Ni, Cu, Mo, the W.
8. the described catalyst of claim 1~3 reduces SO simultaneously at CO 2With the application among the NO, above-mentioned catalytic reduction catalysts is placed reactor, feed CO, SO 2The reaction gas of forming with NO reacts.Wherein reaction temperature is 320~350 ℃, and reaction velocity is 5000h -1~20000h -1
9. according to the described application of claim 8, it is characterized in that described catalyst in the presence of sulfurous gas, carried out presulfurization before using under 400~600 ℃, described sulfurous gas is H 2S, SO 2/ CO or SO 2/ H 2
CN2009101881570A 2009-10-27 2009-10-27 Catalyst for simultaneously reducing SO2 and NO with CO as well as preparation and application of catalyst CN102049257B (en)

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CN102962064A (en) * 2012-11-16 2013-03-13 北京石油化工学院 Gamma-form alumina loaded metallic oxide catalyst as well as preparation method and application thereof
CN102962055A (en) * 2012-11-22 2013-03-13 中节能六合天融环保科技有限公司 Molybdenum-based low-temperature denitration catalyst and preparation thereof
CN103433033A (en) * 2013-07-25 2013-12-11 上海电力学院 Low-temperature denitration catalyst MnOx-CeO2-TiO2-Al2O3, and preparation method and application thereof
CN103464154A (en) * 2013-08-29 2013-12-25 北京石油化工学院 Catalyst for simultaneous catalytic reduction of both NO and SO2 through CO and preparation method and application of catalyst
CN103480273A (en) * 2013-09-30 2014-01-01 东南大学 Highly-activity sodium-based solid carbon dioxide absorbent
CN103566948A (en) * 2013-07-25 2014-02-12 上海电力学院 Low-temperature denitration MnOx-CuO-TiO2-Al2O3 catalyst as well as preparation method and application thereof
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CN104707475A (en) * 2015-04-03 2015-06-17 中南大学 Flue gas treatment method for simultaneous low-temperature photocatalytic self oxidation reduction, desulfurization and denitrification
CN106807346A (en) * 2016-12-30 2017-06-09 洛阳中超新材料股份有限公司 A kind of denitration catalyst carrier and preparation method thereof and denitrating catalyst
CN106955712A (en) * 2017-03-10 2017-07-18 华南师范大学 A kind of Fe Ce based composite catalysts for being applied to vulcanization hydrogen catalysis reduction and desulfurization denitrating technique and preparation method thereof
CN107175108A (en) * 2017-07-10 2017-09-19 中国科学院过程工程研究所 A kind of cobalt series catalyst that sulphur processed is reduced for sulfur dioxide in flue gas and its production and use
CN107398283A (en) * 2017-06-23 2017-11-28 清华大学 Catalyst metals heating surface of NOx content and preparation method thereof in a kind of reduction flue gas
CN107497432A (en) * 2017-08-23 2017-12-22 萍乡市华星化工设备填料有限公司 Efficient cryogenic desulphurization denitration catalyst in coal tar kiln gas

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US5853684A (en) * 1995-11-14 1998-12-29 The Hong Kong University Of Science & Technology Catalytic removal of sulfur dioxide from flue gas
CN1209176C (en) * 2000-09-07 2005-07-06 北京大学 Composite oxide catalyst for eliminating SO2 and NOx in gas mixture simultaneously
CN1107536C (en) * 2000-09-07 2003-05-07 北京大学 Catalyst for eliminating SO2 and NoX in gas mixture simultaneously

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CN102962064A (en) * 2012-11-16 2013-03-13 北京石油化工学院 Gamma-form alumina loaded metallic oxide catalyst as well as preparation method and application thereof
CN102962055A (en) * 2012-11-22 2013-03-13 中节能六合天融环保科技有限公司 Molybdenum-based low-temperature denitration catalyst and preparation thereof
CN103877988B (en) * 2012-12-20 2016-04-27 大连凯特利催化工程技术有限公司 A kind of wide-temperature high-efficiency ammine selectivity catalytic reduction removes NO xcatalysts and its preparation method
CN103877988A (en) * 2012-12-20 2014-06-25 大连凯特利催化工程技术有限公司 Wide-temperature high-efficiency catalyst for NOx removal by ammonia selective catalytic reduction ]and preparation method thereof
CN103433033A (en) * 2013-07-25 2013-12-11 上海电力学院 Low-temperature denitration catalyst MnOx-CeO2-TiO2-Al2O3, and preparation method and application thereof
CN103566948A (en) * 2013-07-25 2014-02-12 上海电力学院 Low-temperature denitration MnOx-CuO-TiO2-Al2O3 catalyst as well as preparation method and application thereof
CN103464154A (en) * 2013-08-29 2013-12-25 北京石油化工学院 Catalyst for simultaneous catalytic reduction of both NO and SO2 through CO and preparation method and application of catalyst
CN103480273A (en) * 2013-09-30 2014-01-01 东南大学 Highly-activity sodium-based solid carbon dioxide absorbent
CN104707475A (en) * 2015-04-03 2015-06-17 中南大学 Flue gas treatment method for simultaneous low-temperature photocatalytic self oxidation reduction, desulfurization and denitrification
CN106807346A (en) * 2016-12-30 2017-06-09 洛阳中超新材料股份有限公司 A kind of denitration catalyst carrier and preparation method thereof and denitrating catalyst
CN106955712A (en) * 2017-03-10 2017-07-18 华南师范大学 A kind of Fe Ce based composite catalysts for being applied to vulcanization hydrogen catalysis reduction and desulfurization denitrating technique and preparation method thereof
CN107398283A (en) * 2017-06-23 2017-11-28 清华大学 Catalyst metals heating surface of NOx content and preparation method thereof in a kind of reduction flue gas
CN107175108A (en) * 2017-07-10 2017-09-19 中国科学院过程工程研究所 A kind of cobalt series catalyst that sulphur processed is reduced for sulfur dioxide in flue gas and its production and use
CN107497432A (en) * 2017-08-23 2017-12-22 萍乡市华星化工设备填料有限公司 Efficient cryogenic desulphurization denitration catalyst in coal tar kiln gas

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