CN101927160A - Catalyst and preparation and application thereof - Google Patents

Catalyst and preparation and application thereof Download PDF

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CN101927160A
CN101927160A CN2009100122648A CN200910012264A CN101927160A CN 101927160 A CN101927160 A CN 101927160A CN 2009100122648 A CN2009100122648 A CN 2009100122648A CN 200910012264 A CN200910012264 A CN 200910012264A CN 101927160 A CN101927160 A CN 101927160A
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catalyst
nitrous oxide
hours
metal
roastings
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田鸣
王晓东
张涛
朱燕燕
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Dalian Institute of Chemical Physics of CAS
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Dalian Institute of Chemical Physics of CAS
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Abstract

The invention relates to a hexaaluminate catalyst used for aerospace propulsion high concentrate nitrous oxide decomposition and a preparation method thereof. By applying the catalyst prepared by the method, nitrous oxide can be spontaneously decomposed under the condition that the temperature is at 450-600 DEG C, the catalyst is endurable to high temperature (1000-1400 DEG C) oxygen enriched fuel gas generated by decomposition of nitrous oxide, and the catalyst has higher activity and high thermo stability on nitrous oxide catalytic decomposition.

Description

A kind of catalyst and preparation thereof and application
Technical field
The present invention relates to a kind of hexa-aluminate catalyzer and preparation method that space flight propulsion high concentration nitrous oxide decomposes that be used for.The catalyst of using this method preparation can make nitrous oxide can realize spontaneous decomposition under 450 ℃～600 ℃ temperature conditions, and can tolerate high temperature (1000 ℃～1400 ℃) oxygen rich fuel gas that nitrous oxide decompose to produce, the catalytic decomposition of nitrous oxide is had greater activity, high thermal stability.
Background technology
In recent years, novel green N 2The O Push Technology has been subjected to great attention at space industry.Main cause is with N 2O advances the novel thrust power of the energy to have himself particular performances.As SP, it can be stored with higher relatively density, and is stored on the spacecraft for a long time as liquid; Its vapour pressure height does not need the rocket body pressure charging system; Nontoxic and with the universal architecture material good compatibility is arranged, this makes does not need too big cost when carrying out systems design and development; The feature of the chemical breakdown heat release that has is applied it on cold air, single constituent element, double elements and the electric resistor heating type thrust chamber of repeatedly igniting.
N 2The catabolite of O is nitrogen and oxygen mixture, reaction equation:
N 2O(g)→N 2(g)+1/2O 2+Heat
Under the standard state, N 2O decomposes the about 82.5kJ/mol of heat that produces, and its pyrolysis activation energy is 250kJ/mol, causes N 2The on-catalytic heat decomposition temperature of O is up to 520 ℃, during practical application for reaching needed thrust (corresponding N 2The O resolution ratio), gaseous state N 2O must be heated to 1000 ℃, and obviously the energy resource system of spacecraft can't satisfy at all.Therefore, must adopt the means of catalytic decomposition to reduce the activation energy that reacts, make N 2O can realize spontaneous decomposition under lower temperature.On the other hand, N 2The catalytic decomposition of O is a strong exothermal reaction, pure N 2The O adiabatic decomposition temperature is up to 1640 ℃, and high temperature will produce strong agglomeration to catalyst again.Therefore, the low-temperature decomposition performance of catalyst and high-temperature stable Journal of Sex Research are space flight propulsion high concentration N 2The primary underlying issue that the O cartalytic decomposition effect is faced.
Carried noble metal is a class catalyst that nitrous oxide is had good catalytic decomposition activity.Discover Ir/Al 2O 3It is one of wherein active best catalyst.But when reaction temperature was higher than 1000 ℃, it is brilliant that alumina support takes place to change, and specific surface area of catalyst obviously reduces; After 1200 ℃～1400 ℃, active component iridium and yttrium oxide generation sintering and volatilization cause the remarkable reduction of catalyst activity, can't continue to use.This seminar had once reported that the hexa-aluminate catalyzer that a kind of novel precious metal iridium replaces was used for high concentration N early stage 2The O decomposition reaction.Yet, because iridium is rare noble metal, costs an arm and a leg, and be senior strategic materials, supply falls short of demand in the international market, and china natural resources has most deficient, makes its application at space industry be subjected to very big restriction.Transition metal is relatively inexpensive, aboundresources.Also do not have at present to be used for space flight propulsion high concentration N about the hexa-aluminate catalyzer of Transition metal substituted 2The relevant report of O decomposition reaction.Therefore, the present invention introduces high concentration N with the hexa-aluminate of Transition metal substituted 2The O cartalytic decomposition effect is to solve above-mentioned N 2O is as problem that missile propellant faced.
Summary of the invention
The present invention relates to a kind of hexa-aluminate catalyzer and preparation and application that space flight propulsion high concentration nitrous oxide decomposes that be used for.The catalyst of using this method preparation can make nitrous oxide can realize spontaneous decomposition under 450 ℃～600 ℃ temperature conditions, and can tolerate high temperature (1000 ℃～1400 ℃) oxygen rich fuel gas that nitrous oxide decompose to produce, the catalytic decomposition of nitrous oxide is had greater activity, high thermal stability.
For achieving the above object, the technical solution used in the present invention is:
Catalyst of the present invention is used for space flight propulsion high concentration nitrous oxide and decomposes.This catalyst is made of carrier and reactive metal two parts.Wherein carrier is hexa-aluminate (AB xAl 12-xO 19, AB xAl 11-xO 17, wherein A represents one or more in alkali metal, alkaline-earth metal, lanthanide series metal, the rare earth metal, and B represents active component).Reactive metal is: the mixture of one or more elements in manganese, iron, cobalt, the copper, reactive metal quality percentage composition is 3%～20%.Catalyst adopts the coprecipitation preparation.
Catalyst described in the present invention adopts the coprecipitation preparation.The nitrate of related metal in the nitrate of reactive metal and the carrier component is dissolved in respectively in 50～80 ℃ an amount of water, to except that aluminum nitrate solution, mix by other solution, regulate pH=1～3, aluminum nitrate solution is added, after mixing, add rapidly in the quantitative saturated sal volatile, stirred 4～6 hours fast, filter the back dried overnight in 50～80 ℃.300～500 ℃ of roastings 2～5 hours, 1200～1400 ℃ of roastings 4～6 hours.
The catalyst of using this method preparation can make nitrous oxide can realize spontaneous decomposition under 450 ℃～600 ℃ temperature conditions, and can tolerate high temperature (1000 ℃～1400 ℃) oxygen rich fuel gas that nitrous oxide decompose to produce, the catalytic decomposition of nitrous oxide is had greater activity, high thermal stability.
Catalyst described in the present invention can be applicable to aspects such as gas generator, attitude of flight vehicle control.
Description of drawings
Fig. 1 is LaMn xAl 12-xO 19And BaMn xAl 12-xO 19Hexa-aluminate crystalline phase spectrogram.As can be seen from the figure catalyst through 1200 ℃ of roastings after, present complete hexa-aluminate crystalline phase, and be mixed with the LaAlO of trace 3Phase.
Fig. 2 is for the embodiment of the invention 2 and relatively implement 2,4,6 temperature programming reaction result comparison diagrams.As can be seen from the figure, the hexa-aluminate catalyzer of manganese replacement shows best N 2The O degrading activity.
Fig. 3 is the embodiment of the invention 4 temperature programming reaction result figure.As can be seen from the figure, when the replacement amount x=1 of manganese, catalyst shows best N 2The O degrading activity.
Fig. 4 is for the embodiment of the invention 4 and relatively implement 8,10,12 temperature programming reaction result comparison diagrams.After 1200 ℃ of roastings, BaMnAl 11O 19Hexa-aluminate catalyzer compares Mn/Al 2O 3Catalyst shows better N 2The O degrading activity.And the body phase manganese in the hexa-aluminate crystalline phase is N 2The main activated centre of O decomposition reaction, and the outer manganese oxide species of hexa-aluminate crystalline phase are contributed less to catalytic performance.
Fig. 5 is the embodiment of the invention 7 stability analyses figure as a result.As can be seen from the figure, through 40 hours N2O decomposition reaction, BaMnAl 11O 19Tangible inactivation does not take place in hexa-aluminate catalyzer, and BaMnAl is described 11O 19Hexa-aluminate catalyzer has excellent high-temperature stability.
Fig. 6 is the reaction result figure of the embodiment of the invention 8 in the time of 650 ℃.As can be seen from the figure, along with the prolongation of roasting time, catalyst activity slightly descends.
The specific embodiment
Following example is used to illustrate in greater detail the present invention, but the present invention is not limited to this.
Embodiment 1
Preparation LaMn xAl 12-xO 19(active material Mn content is 7% to catalyst; As follows): with lanthanum nitrate (La (NO 3) 3.6H 2O) 1.1g, manganese nitrate (50%aq) 0.9g, and aluminum nitrate (Al (NO 3) 3.9H 2O) 10.3g is dissolved in respectively in the deionized water of 60 ℃ of 20ml, will mix by other solution except that aluminum nitrate solution, regulates pH=1, aluminum nitrate solution is added, after mixing, add rapidly in the saturated sal volatile of 150ml, stirred 6 hours fast in 60 ℃, filter the back dried overnight.500 ℃ of roastings 2 hours, 1200 ℃ of roastings 4 hours.
Embodiment 2
Under the room temperature condition, getting granularity is 40～60 order LaMn xAl 12-xO 19Catalyst 100mg places the straight tube reactor, and air speed is 30,000ml g -1h -1, 5 ℃/min temperature programming behind each temperature spot constant temperature 40min to be measured, is formed with chromatogram detection reaction device exit gas, and calculates conversion ratio.Evaluation result as shown in Figure 2.
Embodiment 3
Preparation BaMn xAl 12-xO 19(with active material Mn content is 7% to be example to catalyst; The method for preparing catalyst of other manganese content is identical): with manganese nitrate (50%aq) 0.9g, barium nitrate (Ba (NO 3) 2) 0.7g and aluminum nitrate (Al (NO 3) 3.9H 2O) 10.3g is dissolved in respectively in the deionized water of 60 ℃ of 20ml, will mix by other solution except that aluminum nitrate solution, regulates pH=1, aluminum nitrate solution is added, after mixing, add rapidly in the saturated sal volatile of 150ml, stirred 6 hours fast in 60 ℃, filter back 120 ℃ of dried overnight.500 ℃ of roastings 2 hours, 1200 ℃ of roastings 4 hours.
Embodiment 4
Under the room temperature condition, getting granularity is 40～60 order BaMn xAl 12-xO 19Catalyst 100mg places the straight tube reactor, and air speed is 30,000ml g -1h -1, 5 ℃/min temperature programming behind each temperature spot constant temperature 40min to be measured, is formed with chromatogram detection reaction device exit gas, and calculates conversion ratio.Evaluation result is shown in Fig. 3 and 4.
Embodiment 5
Preparation BaCo xAl 12-xO 19(active material Co content is 7% to catalyst; As follows): with cobalt nitrate (Co (NO 3) .6H 2O) 0.7g, barium nitrate (Ba (NO 3) 2) 0.7g and aluminum nitrate (Al (NO 3) 3.9H 2O) 10.3g is dissolved in respectively in the deionized water of 60 ℃ of 20ml, will mix by other solution except that aluminum nitrate solution, regulates pH=1, aluminum nitrate solution is added, after mixing, add rapidly in the saturated sal volatile of 150ml, stirred 6 hours fast in 60 ℃, filter back 120 ℃ of dried overnight.500 ℃ of roastings 2 hours, 1200 ℃ of roastings 4 hours.
Embodiment 6
Preparation BaCu xAl 12-xO 19(active material Cu content is 5% to catalyst; As follows): with copper nitrate (Cu (NO 3) 2.3H 2O) 0.6g, barium nitrate (Ba (NO 3) 2) 0.7g and aluminum nitrate (Al (NO 3) 3.9H 2O) 10.3g is dissolved in respectively in the deionized water of 60 ℃ of 20ml, will mix by other solution except that aluminum nitrate solution, regulates pH=1, aluminum nitrate solution is added, after mixing, add rapidly in the saturated sal volatile of 150ml, stirred 6 hours fast in 60 ℃, filter back 120 ℃ of dried overnight.500 ℃ of roastings 2 hours, 1200 ℃ of roastings 4 hours.
Comparing embodiment 1
Preparation LaFe xAl 12-xO 19(active material Fe content is 7% to catalyst; As follows): with ferric nitrate (Fe (NO 3) .9H 2O) 1.0g, barium nitrate (Ba (NO 3) 2) 1.1g and aluminum nitrate (Al (NO 3) 3.9H 2O) 10.3g is dissolved in respectively in the deionized water of 60 ℃ of 20ml, to except that aluminum nitrate solution, mix by other solution, regulate pH=1～3, aluminum nitrate solution is added, after mixing, add rapidly in the saturated sal volatile of 150ml, stirred 6 hours fast, filter back 120 ℃ of dried overnight in 60 ℃.500 ℃ of roastings 2 hours, 1200 ℃ of roastings 4 hours.
Comparing embodiment 2
Under the room temperature condition, getting granularity is 40～60 order LaFe xAl 12-xO 19Catalyst 100mg places the straight tube reactor, and air speed is 30,000ml g -1h -1, 5 ℃/min temperature programming behind each temperature spot constant temperature 40min to be measured, is formed with chromatogram detection reaction device exit gas, and calculates conversion ratio.Evaluation result as shown in Figure 2.
Comparing embodiment 3
Preparation LaCo xAl 12-xO 19Catalyst: with cobalt nitrate (Co (NO 3) .6H 2O) 0.7g, lanthanum nitrate (La (NO 3) 2) 1.1g and aluminum nitrate (Al (NO 3) 3.9H 2O) 10.3g is dissolved in respectively in the deionized water of 60 ℃ of 20ml, will mix by other solution except that aluminum nitrate solution, regulates pH=1, aluminum nitrate solution is added, after mixing, add rapidly in the saturated sal volatile of 150ml, stirred 6 hours fast in 60 ℃, filter back 120 ℃ of dried overnight.500 ℃ of roastings 2 hours, 1200 ℃ of roastings 4 hours.
Comparing embodiment 4
Under the room temperature condition, getting granularity is 40～60 order LaCo xAl 12-xO 19Catalyst 100mg places the straight tube reactor, and air speed is 30,000ml g -1h -1, 5 ℃/min temperature programming behind each temperature spot constant temperature 40min to be measured, is formed with chromatogram detection reaction device exit gas, and calculates conversion ratio.Evaluation result as shown in Figure 2.
Comparing embodiment 5
Preparation LaCu xAl 12-xO 19Catalyst: with copper nitrate (Cu (NO 3) 2.3H 2O) 0.6g, lanthanum nitrate (La (NO 3) 3.6H 2O) 1.1g and aluminum nitrate (Al (NO 3) 3.9H 2O) 10.3g is dissolved in respectively in the deionized water of 60 ℃ of 20ml, will mix by other solution except that aluminum nitrate solution, regulates pH=1, aluminum nitrate solution is added, after mixing, add rapidly in the saturated sal volatile of 150ml, stirred 6 hours fast in 60 ℃, filter back 120 ℃ of dried overnight.500 ℃ of roastings 2 hours, 1200 ℃ of roastings 4 hours.
Comparing embodiment 6
Under the room temperature condition, getting granularity is 40～60 order LaCu xAl 12-xO 19Catalyst 100mg places the straight tube reactor, and air speed is 30,000ml g -1h -1, 5 ℃/min temperature programming behind each temperature spot constant temperature 40min to be measured, is formed with chromatogram detection reaction device exit gas, and calculates conversion ratio.Evaluation result as shown in Figure 2.
Comparing embodiment 7
Under the room temperature condition, prepare 7wt%Mn/Al with coprecipitation 2O 3Catalyst.With manganese nitrate (50%aq) 0.9g and aluminum nitrate (Al (NO 3) 3.9H 2O) 7.5g is dissolved in respectively in the deionized water of 60 ℃ of 20ml, after mixing, adds rapidly in the saturated sal volatile of 100ml, stirs 6 hours fast in 60 ℃, filters back 120 ℃ of dried overnight.500 ℃ of roastings 2 hours, 1200 ℃ of roastings 4 hours.
Comparing embodiment 8
Under the room temperature condition, getting granularity is the 7wt%Mn/Al of 40～60 order coprecipitations preparation 2O 3Catalyst 100mg places the straight tube reactor, and air speed is 30,000ml g -1h -1, 5 ℃/min temperature programming behind each temperature spot constant temperature 40min to be measured, is formed with chromatogram detection reaction device exit gas, and calculates conversion ratio.Evaluation result as shown in Figure 4.
Comparing embodiment 9
Preparation BaAl 12O 19Catalyst.With barium nitrate (Ba (NO 3) 2) 0.7g and aluminum nitrate (Al (NO 3) 3.9H 2O) 11.3g is dissolved in respectively in the deionized water of 60 ℃ of 20ml, will mix by other solution except that aluminum nitrate solution, regulates pH=1, aluminum nitrate solution is added, after mixing, add rapidly in the saturated sal volatile of 100ml, stirred 6 hours fast in 60 ℃, filter back 120 ℃ of dried overnight.500 ℃ of roastings 2 hours, 1200 ℃ of roastings 4 hours.
Comparing embodiment 10
Under the room temperature condition, getting granularity is 40～60 order BaAl 12O 19Catalyst 100mg places the straight tube reactor, and air speed is 30,000ml g -1h -1, 5 ℃/min temperature programming behind each temperature spot constant temperature 40min to be measured, is formed with chromatogram detection reaction device exit gas, and calculates conversion ratio.Evaluation result as shown in Figure 4.
Comparing embodiment 11
Preparation support type 7wt%Mn/BaAl 12O 19Catalyst.BaAl with the preparation of comparing embodiment 3 methods 12O 19, adopt equi-volume impregnating to introduce manganese, preparation Mn/BaAl 12O 19Catalyst, 80 ℃ of dried overnight, 500 ℃ of roastings 2 hours.
Comparing embodiment 12
Under the room temperature condition, getting granularity is 40～60 order 7wt%Mn/BaAl 12O 19Catalyst 100mg places the straight tube reactor, and air speed is 30,000ml g -1h -1, 5 ℃/min temperature programming behind each temperature spot constant temperature 40min to be measured, is formed with chromatogram detection reaction device exit gas, and calculates conversion ratio.Evaluation result as shown in Figure 4.
Embodiment 7
Stability test.Under the room temperature condition, getting granularity is 40～60 order 7wt%BaMn xAl 12-xO 19Catalyst 100mg places the straight tube reactor, and air speed is 30,000ml g -1h -1, 5 ℃/min temperature programming to 800 ℃ behind each temperature spot constant temperature 40min to be measured, is formed with chromatogram detection reaction device exit gas, and calculates conversion ratio.Evaluation result as shown in Figure 5.
Embodiment 8
The high heat stability property testing.With 7wt%BaMn xAl 12-xO 19Hexa-aluminate was distinguished roasting after 4,6,8,10 hours under 1200 ℃ of air atmospheres, under the room temperature condition, getting granularity is 40～60 order BaMn xAl 12-xO 19-t (t is 1200 ℃ a roasting time, t=4,6,8,10) catalyst 100mg places the straight tube reactor, and air speed is 30,000ml g -1h -1, 5 ℃/min temperature programming to 800 ℃ behind each temperature spot constant temperature 40min to be measured, is formed with chromatogram detection reaction device exit gas, and calculates conversion ratio.Evaluation result as shown in Figure 6.

Claims (4)

1. catalyst, this catalyst is made of carrier and reactive metal two parts, and wherein carrier is a hexa-aluminate, and reactive metal is the mixture of one or more elements in manganese, iron, cobalt, the copper, and reactive metal quality percentage composition is 3%～20%.
2. according to the described catalyst of claim 1, it is characterized in that: the structural group of described catalyst becomes, AB xAl 12-xO 19Or AB xAl 11-xO 17, wherein A represents one or more in alkali metal, alkaline-earth metal, lanthanide series metal, the rare earth metal, and B represents active component, x=0.5,1,2 or 3.
3. described Preparation of catalysts method of claim 1, it is characterized in that: described catalyst adopts the coprecipitation preparation, the nitrate of related metal in the nitrate of reactive metal and the carrier component is dissolved in respectively in 50～80 ℃ the water, to except that aluminum nitrate solution, mix by other solution, regulate pH=1～3, then aluminum nitrate solution be added, after mixing, add rapidly in the quantitative saturated sal volatile, stirred 4～6 hours fast, filter the back dried overnight in 50～80 ℃; 300～500 ℃ of roastings 2～5 hours, 1200～1400 ℃ of roastings 4～6 hours.
4. Application of Catalyst described in the claim 1, it is characterized in that: described catalyst is used for nitrous oxide 450～600 ℃ of spontaneous decomposition, and it has the high de-agglomeration activity to space flight propulsion high concentration nitrous oxide; Can tolerate 1000 ℃～1400 ℃ high-temperature oxygen-enriched combustion gas that nitrous oxide decompose to produce, the decomposition of space flight propulsion high concentration nitrous oxide is had high thermal stability.
CN2009100122648A 2009-06-26 2009-06-26 Catalyst and preparation and application thereof Pending CN101927160A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102861585A (en) * 2011-07-07 2013-01-09 中国科学院大连化学物理研究所 Space propulsion level nitrogen monoxide decomposed catalyst and preparation method and application thereof
EP2812111A4 (en) * 2012-02-10 2015-11-18 Basf Se Hexaaluminate-comprising catalyst for reforming of hydrocarbons and reforming process
US9566571B2 (en) 2012-02-10 2017-02-14 Basf Se Hexaaluminate-comprising catalyst for the reforming of hydrocarbons and a reforming process
CN113600202A (en) * 2021-09-09 2021-11-05 上海华峰新材料研发科技有限公司 Catalyst for decomposing nitrous oxide, preparation method thereof and nitrous oxide decomposition method
CN114832615A (en) * 2022-04-01 2022-08-02 开滦能源化工股份有限公司 Method and device for catalyzing decomposition of nitrous oxide
CN115228456A (en) * 2021-12-17 2022-10-25 中国石油天然气股份有限公司 High-efficiency catalyst for catalytic decomposition of nitrous oxide

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
SHAOMIN ZHU ET AL.: "Superior performance of Ir-substituted hexaaluminate catalysts for N2O decomposition", 《CATALYSIS TODAY》 *
董留涛等: "LaCuxZn1-xAl11O19-δ六铝酸盐催化剂分解N2O的催化性能", 《环境化学》 *

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102861585A (en) * 2011-07-07 2013-01-09 中国科学院大连化学物理研究所 Space propulsion level nitrogen monoxide decomposed catalyst and preparation method and application thereof
EP2812111A4 (en) * 2012-02-10 2015-11-18 Basf Se Hexaaluminate-comprising catalyst for reforming of hydrocarbons and reforming process
US9566571B2 (en) 2012-02-10 2017-02-14 Basf Se Hexaaluminate-comprising catalyst for the reforming of hydrocarbons and a reforming process
US10987660B2 (en) 2012-02-10 2021-04-27 Basf Se Hexaaluminate-comprising catalyst for the reforming of hydrocarbons and a reforming process
CN113600202A (en) * 2021-09-09 2021-11-05 上海华峰新材料研发科技有限公司 Catalyst for decomposing nitrous oxide, preparation method thereof and nitrous oxide decomposition method
CN113600202B (en) * 2021-09-09 2023-09-01 上海华峰新材料研发科技有限公司 Catalyst for decomposing nitrous oxide, preparation method thereof and decomposition method of nitrous oxide
CN115228456A (en) * 2021-12-17 2022-10-25 中国石油天然气股份有限公司 High-efficiency catalyst for catalytic decomposition of nitrous oxide
CN114832615A (en) * 2022-04-01 2022-08-02 开滦能源化工股份有限公司 Method and device for catalyzing decomposition of nitrous oxide

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Application publication date: 20101229