CN107051469A - One kind is based on hydrogenation of carbon dioxide producing light olefins composite catalyst and preparation method thereof - Google Patents
One kind is based on hydrogenation of carbon dioxide producing light olefins composite catalyst and preparation method thereof Download PDFInfo
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- CN107051469A CN107051469A CN201710214395.9A CN201710214395A CN107051469A CN 107051469 A CN107051469 A CN 107051469A CN 201710214395 A CN201710214395 A CN 201710214395A CN 107051469 A CN107051469 A CN 107051469A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/889—Manganese, technetium or rhenium
- B01J23/8892—Manganese
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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- C—CHEMISTRY; METALLURGY
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- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C1/00—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon
- C07C1/02—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon from oxides of a carbon
- C07C1/12—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon from oxides of a carbon from carbon dioxide with hydrogen
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2523/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00
- C07C2523/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00 of the iron group metals or copper
- C07C2523/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups C07C2523/02 - C07C2523/36
- C07C2523/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups C07C2523/02 - C07C2523/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- C07C2523/889—Manganese, technetium or rhenium
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Abstract
Hydrogenation of carbon dioxide producing light olefins composite catalyst and preparation method thereof is based on the invention discloses one kind of energy-conserving and environment-protective technical fiel, following weight should be pressed based on hydrogenation of carbon dioxide producing light olefins composite catalyst：Zr(NO3)4·5H2O：40~60 parts；NH3·H2O：5~7 parts；NaOH：80~100 parts；NaAlO2：70~90 parts；Al2(SO4)3：30~50 parts；Fe(NO3)3·9H2O：40~50 parts；CO(NH2)2：10~15 parts；Reaction promoter：3~5 parts, operating method of the present invention is simple, and the light olefins catalyst activity of preparation is high, and reducing property is good, and stability is strong, is adapted to the production in enormous quantities of factory.
Description
Technical field
It is specially that a kind of be combined based on hydrogenation of carbon dioxide producing light olefins is urged the present invention relates to energy-conserving and environment-protective technical fiel
Agent and preparation method thereof.
Background technology
The energy is human social development and progressive essential power, and China is a populous nation, while being also energy
Big country is consumed in source, adds that economic development is more and more faster, and the demand to the energy is also increasing.The energy consumed in the world at present
Predominantly fossil fuel, including crude oil, raw coal and natural gas etc..These energy are all the non-renewable energy, and are distributed non-
It is often unbalanced.The petroleum reserves in the Persian Gulf, north African and the Gulf of Mexico accounts for the 51.3% of world oil gross reserves, for country,
Petroleum reserves at most be Saudi Arabia, account for the 21.9% of world oil gross reserves, and the petroleum reserves of China only has the 6% of Saudi Arabia,
It is ranked first in the world 3.Natural gas is mainly distributed on Europe and Russia, and Russian gas reserves at most, accounts for the world
The 26.3% of natural gas gross reserves, the gas reserves of China is then fewer.The coal annual production of China accounts for the second in the world, simultaneously
It is also to consume the most country of coal every year in the world, because the coal resources quality of China is not universal high, sulfur content is higher, mesh
Preceding China is also to pollute one of more serious country in the world.It is how sharp for the current energy source distribution of China and service condition
With the coal resources of China's abundant, the path for seeking a kind of replacement oil of high-efficiency cleaning is extremely urgent.Therefore, we carry
Go out a kind of hydrogenation of carbon dioxide producing light olefins composite catalyst and preparation method thereof that is based on to come into operation, to solve above-mentioned ask
Topic.
The content of the invention
Hydrogenation of carbon dioxide producing light olefins composite catalyst and its preparation are based on it is an object of the invention to provide one kind
Method, to solve the problems mentioned in the above background technology.
To achieve the above object, the present invention provides following technical scheme：One kind is based on hydrogenation of carbon dioxide producing light olefins
Composite catalyst, should press following weight based on hydrogenation of carbon dioxide producing light olefins composite catalyst：
Zr(NO3)4·5H2O：40~60 parts；
NH3·H2O：5~7 parts；
NaOH：80~100 parts；
NaAlO2：70~90 parts；
Al2(SO4)3：30~50 parts；
Fe(NO3)3·9H2O：40~50 parts；
CO(NH2)2：10~15 parts；
Reaction promoter：3~5 parts.
It is preferred that, the reaction promoter is that can reduce CH4The Mn structural promoters of content.
It is preferred that, a kind of preparation method based on hydrogenation of carbon dioxide producing light olefins composite catalyst should be based on dioxy
Change carbon is hydrogenated with comprising the following steps that for the preparation method of producing light olefins composite catalyst：
S1：By 40~60 parts of Zr (NO3)4·5H2O is configured to 1~3mol/L solution, and 5 are added dropwise under conditions of stirring
~7 parts of NH3·H2Zr (OH) is obtained after O4Sediment, and by Zr (OH)4It is washed with deionized standby after filtering；
S2：By 80~100 parts of NaOH and 70~90 part of NaAlO2Mixed liquor is formed in the water for being dissolved in 400~600ml,
It is slowly added dropwise after stirring in mixed liquor to 7~9g Ludox, quick stirring and at room temperature 10~12h of aging；
S3：Mixed solution in step S2 is transferred in reactor, and poured into reactor obtained in step S1
Zr(OH)4, it is heat-treated 72h under conditions of 180~200 DEG C, and catalyst aid is made after washing 3~5 times；
S4：By 30~50 parts of Al2(SO4)3Al is formed in the deionized water for being dissolved in 100~150ml2(SO4)3Solution, will
40~50 parts of Fe (NO3)3·9H2O, which is dissolved in 100~150ml deionized water, forms Fe (NO3)3·9H2O solution, in stirring
Under the conditions of Al2(SO4)3Solution is slowly added to Fe (NO3)3·9H2Mixed solution, and the side in mixed solution are formed in O solution
Stirring side is slowly dropped into 7~9g Ludox；
S5：Added in mixed solution made from step S4 after obtained catalyst aid in step S3,30~35min of stirring
10~15 parts of CO (NH are slowly added again2)2, 3~5 parts of reaction promoter continuation stirring is then added until reaction promoter is complete
Dissolving；
S6：Mixed solution in step S5 is moved into reactor, used at 180~200 DEG C after 3~5d of crystallization, cooling
Deionized water is washed till PH=8, and light olefins catalyst is obtained after drying, roasting.
It is preferred that, in the step S2, Ludox is by Na2O、SiO2、Al2O3And H2O is constituted, and Na2O：SiO2：Al2O3：
H2O=14:80:6:1800.
It is preferred that, in the step S4, in whipping process, first by the circle of stirring 3~5 clockwise after, to stir counterclockwise
3~5 circles are mixed, untill Ludox and mixed solution are thoroughly mixed.
It is preferred that, in the step S6,400~750 DEG C of sintering temperature, roasting time is 1~1.5h.
Compared with prior art, the beneficial effects of the invention are as follows：Operating method of the present invention is simple, and the low-carbon alkene of preparation is urged
Agent activity is high, and reducing property is good, and stability is strong, is adapted to the production in enormous quantities of factory.
Brief description of the drawings
Fig. 1 is workflow diagram of the present invention；
Fig. 2 is the vibrational band figure of the present invention different crystallization times under the conditions of 190 DEG C.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation is described, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments.It is based on
Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under the premise of creative work is not made
Embodiment, belongs to the scope of protection of the invention.
Embodiment one
One kind is based on hydrogenation of carbon dioxide producing light olefins composite catalyst, should be based on hydrogenation of carbon dioxide producing light olefins
Composite catalyst presses following weight：
Zr(NO3)4·5H2O：40 parts；
NH3·H2O：5 parts；
NaOH：80 parts；
NaAlO2：70 parts；
Al2(SO4)3：30 parts；
Fe(NO3)3·9H2O：40 parts；
CO(NH2)2：10 parts；
Reaction promoter：3 parts, reaction promoter is that can reduce CH4The Mn structural promoters of content.
Present invention also offers a kind of preparation method based on hydrogenation of carbon dioxide producing light olefins composite catalyst, the base
Comprised the following steps that in the preparation method of hydrogenation of carbon dioxide producing light olefins composite catalyst：
S1：By 40 parts of Zr (NO3)4·5H2O is configured to 1~3mol/L solution, and 5 parts are added dropwise under conditions of stirring
NH3·H2Zr (OH) is obtained after O4Sediment, and by Zr (OH)4It is washed with deionized standby after filtering；
S2：By 80 parts of NaOH and 70 part of NaAlO2Mixed liquor is formed in the water for being dissolved in 400ml, mixed after stirring
Close and be slowly added dropwise in liquid to 7g Ludox, quick stirring and at room temperature aging 10h, Ludox is by Na2O、SiO2、Al2O3And H2O
Composition, and Na2O：SiO2：Al2O3：H2O=14:80:6:1800；
S3：Mixed solution in step S2 is transferred in reactor, and poured into reactor obtained in step S1
Zr(OH)4, it is heat-treated 72h under conditions of 180 DEG C, and catalyst aid is made after washing 3 times；
S4：By 30 parts of Al2(SO4)3Al is formed in the deionized water for being dissolved in 100~150ml2(SO4)3Solution, by 40 parts
Fe (NO3)3·9H2O, which is dissolved in 100~150ml deionized water, forms Fe (NO3)3·9H2O solution, under agitation
Al2(SO4)3Solution is slowly added to Fe (NO3)3·9H2Mixed solution is formed in O solution, and is delayed while stirring in mixed solution
It is slow to instill 7g Ludox, in whipping process, after first being enclosed by stirring 3 clockwise, enclosed to stir 3 counterclockwise, until Ludox
Untill being thoroughly mixed with mixed solution；
S5：Delay again after obtained catalyst aid in step S3, stirring 30min are added in mixed solution made from step S4
CO (the NH of slow 10 parts of addition2)2, the reaction promoter continuation stirring of then 3 parts of addition is until reaction promoter is completely dissolved；
S6：Mixed solution in step S5 is moved into reactor, deionized water is used after crystallization 4d, cooling at 180 DEG C
PH=8 is washed till, light olefins catalyst is obtained after drying, roasting, 400 DEG C of sintering temperature, roasting time is 1h.
Embodiment two
One kind is based on hydrogenation of carbon dioxide producing light olefins composite catalyst, should be based on hydrogenation of carbon dioxide producing light olefins
Composite catalyst presses following weight：
Zr(NO3)4·5H2O：60 parts；
NH3·H2O：7 parts；
NaOH：100 parts；
NaAlO2：90 parts；
Al2(SO4)3：50 parts；
Fe(NO3)3·9H2O：50 parts；
CO(NH2)2：15 parts；
Reaction promoter：5 parts, reaction promoter is that can reduce CH4The Mn structural promoters of content.
Present invention also offers a kind of preparation method based on hydrogenation of carbon dioxide producing light olefins composite catalyst, the base
Comprised the following steps that in the preparation method of hydrogenation of carbon dioxide producing light olefins composite catalyst：
S1：By 60 parts of Zr (NO3)4·5H2O is configured to 1~3mol/L solution, and 7 parts are added dropwise under conditions of stirring
NH3·H2Zr (OH) is obtained after O4Sediment, and by Zr (OH)4It is washed with deionized standby after filtering；
S2：By 100 parts of NaOH and 90 part of NaAlO2Form mixed liquor in the water for being dissolved in 600ml, after stirring
It is slowly added dropwise in mixed liquor to 9g Ludox, quick stirring and at room temperature aging 12h, Ludox is by Na2O、SiO2、Al2O3With
H2O is constituted, and Na2O：SiO2：Al2O3：H2O=14:80:6:1800；
S3：Mixed solution in step S2 is transferred in reactor, and poured into reactor obtained in step S1
Zr(OH)4, it is heat-treated 72h under conditions of 200 DEG C, and catalyst aid is made after washing 5 times；
S4：By 50 parts of Al2(SO4)3Al is formed in the deionized water for being dissolved in 150ml2(SO4)3Solution, by 50 parts of Fe
(NO3)3·9H2O, which is dissolved in 150ml deionized water, forms Fe (NO3)3·9H2O solution, under agitation Al2(SO4)3
Solution is slowly added to Fe (NO3)3·9H2Mixed solution is formed in O solution, and is slowly dropped into mixed solution 9g while stirring
Ludox, in whipping process, after first being enclosed by stirring 5 clockwise, is enclosed, until Ludox is molten with mixing to stir 5 counterclockwise
Untill liquid is thoroughly mixed；
S5：Delay again after obtained catalyst aid in step S3, stirring 35min are added in mixed solution made from step S4
CO (the NH of slow 15 parts of addition2)2, the reaction promoter continuation stirring of then 5 parts of addition is until reaction promoter is completely dissolved；
S6：Mixed solution in step S5 is moved into reactor, deionized water is used after crystallization 5d, cooling at 200 DEG C
PH=8 is washed till, light olefins catalyst is obtained after drying, roasting, 750 DEG C of sintering temperature, roasting time is 1.5h.
Embodiment three
One kind is based on hydrogenation of carbon dioxide producing light olefins composite catalyst, should be based on hydrogenation of carbon dioxide producing light olefins
Composite catalyst presses following weight：
Zr(NO3)4·5H2O：50 parts；
NH3·H2O：6 parts；
NaOH：90 parts；
NaAlO2：80 parts；
Al2(SO4)3：40 parts；
Fe(NO3)3·9H2O：45 parts；
CO(NH2)2：135 parts；
Reaction promoter：4 parts, reaction promoter is that can reduce CH4The Mn structural promoters of content.
Present invention also offers a kind of preparation method based on hydrogenation of carbon dioxide producing light olefins composite catalyst, the base
Comprised the following steps that in the preparation method of hydrogenation of carbon dioxide producing light olefins composite catalyst：
S1：By 50 parts of Zr (NO3)4·5H2O is configured to 1~3mol/L solution, and 6 parts are added dropwise under conditions of stirring
NH3·H2Zr (OH) is obtained after O4Sediment, and by Zr (OH)4It is washed with deionized standby after filtering；
S2：By 90 parts of NaOH and 80 part of NaAlO2Mixed liquor is formed in the water for being dissolved in 500ml, mixed after stirring
Close and be slowly added dropwise in liquid to 8g Ludox, quick stirring and at room temperature aging 11h, Ludox is by Na2O、SiO2、Al2O3And H2O
Composition, and Na2O：SiO2：Al2O3：H2O=14:80:6:1800；
S3：Mixed solution in step S2 is transferred in reactor, and poured into reactor obtained in step S1
Zr(OH)4, it is heat-treated 72h under conditions of 190 DEG C, and catalyst aid is made after washing 4 times；
S4：By 40 parts of Al2(SO4)3Al is formed in the deionized water for being dissolved in 130ml2(SO4)3Solution, by 45 parts of Fe
(NO3)3·9H2O, which is dissolved in 130ml deionized water, forms Fe (NO3)3·9H2O solution, under agitation Al2(SO4)3
Solution is slowly added to Fe (NO3)3·9H2Mixed solution is formed in O solution, and is slowly dropped into mixed solution 8g while stirring
Ludox, in whipping process, after first being enclosed by stirring 4 clockwise, is enclosed, until Ludox is molten with mixing to stir 4 counterclockwise
Untill liquid is thoroughly mixed；
S5：Delay again after obtained catalyst aid in step S3, stirring 33min are added in mixed solution made from step S4
CO (the NH of slow 13 parts of addition2)2, the reaction promoter continuation stirring of then 4 parts of addition is until reaction promoter is completely dissolved；
S6：Mixed solution in step S5 is moved into reactor, deionized water is used after crystallization 3d, cooling at 190 DEG C
PH=8 is washed till, light olefins catalyst is obtained after drying, roasting, 600 DEG C of sintering temperature, roasting time is 1.3h.
Referring to Fig. 2, being less than 1250cm in figure-1Vibrating area be skeleton fundamental vibration area, vibration peak peak position is in 1369cm-1The sum of fundamental frequencies of neighbouring skeletal vibration or general frequency band, in 3460cm-1Surface hydroxyl and adsorb shaking for water that neighbouring vibration peak is represented
It is dynamic, 450cm-1Neighbouring vibration peak represents its internal tetrahedron vibration, and when crystallization time is 3d, crystallization temperature is to synthesis
The crystallinity of light olefins catalyst has a great impact, when crystallization temperature is less than 190 degrees Celsius, with the liter of crystallization temperature
Height, the skeleton structure of low-carbon alkene tends to balance, and tends to perfect, in summary described, of the invention optimal reality during to 190 DEG C
Example is applied for embodiment three.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of changes, modification can be carried out to these embodiments, replace without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (6)
1. one kind is based on hydrogenation of carbon dioxide producing light olefins composite catalyst, it is characterised in that：Hydrogenation of carbon dioxide should be based on
Producing light olefins composite catalyst presses following weight：
Zr(NO3)4·5H2O：40~60 parts；
NH3·H2O：5~7 parts；
NaOH：80~100 parts；
NaAlO2：70~90 parts；
Al2(SO4)3：30~50 parts；
Fe(NO3)3·9H2O：40~50 parts；
CO(NH2)2：10~15 parts；
Reaction promoter：3~5 parts.
2. it is according to claim 1 a kind of based on hydrogenation of carbon dioxide producing light olefins composite catalyst, it is characterised in that：
The reaction promoter is that can reduce CH4The Mn structural promoters of content.
3. a kind of preparation method based on hydrogenation of carbon dioxide producing light olefins composite catalyst, it is characterised in that：Two should be based on
Carbonoxide is hydrogenated with comprising the following steps that for the preparation method of producing light olefins composite catalyst：
S1：By 40~60 parts of Zr (NO3)4·5H2O is configured to 1~3mol/L solution, and 5~7 are added dropwise under conditions of stirring
The NH of part3·H2Zr (OH) is obtained after O4Sediment, and by Zr (OH)4It is washed with deionized standby after filtering；
S2：By 80~100 parts of NaOH and 70~90 part of NaAlO2Mixed liquor is formed in the water for being dissolved in 400~600ml, is stirred
It is slowly added dropwise after uniform in mixed liquor to 7~9g Ludox, quick stirring and at room temperature 10~12h of aging；
S3：Mixed solution in step S2 is transferred in reactor, and pours into reactor obtained Zr in step S1
(OH)4, it is heat-treated 72h under conditions of 180~200 DEG C, and catalyst aid is made after washing 3~5 times；
S4：By 30~50 parts of Al2(SO4)3Al is formed in the deionized water for being dissolved in 100~150ml2(SO4)3Solution, by 40~
50 parts of Fe (NO3)3·9H2O, which is dissolved in 100~150ml deionized water, forms Fe (NO3)3·9H2O solution, in stirring condition
It is lower Al2(SO4)3Solution is slowly added to Fe (NO3)3·9H2Mixed solution is formed in O solution, and side is stirred in mixed solution
While being slowly dropped into 7~9g Ludox；
S5：Delay again after obtained catalyst aid in step S3,30~35min of stirring are added in mixed solution made from step S4
CO (the NH of slow 10~15 parts of addition2)2, 3~5 parts of reaction promoter continuation stirring is then added until reaction promoter is completely dissolved；
S6：Mixed solution in step S5 is moved into reactor, spent at 180~200 DEG C after 3~5d of crystallization, cooling from
Son is washed to PH=8, and light olefins catalyst is obtained after drying, roasting.
4. a kind of preparation method based on hydrogenation of carbon dioxide producing light olefins composite catalyst according to claim 3,
It is characterized in that：In the step S2, Ludox is by Na2O、SiO2、Al2O3And H2O is constituted, and Na2O：SiO2：Al2O3：H2O=
14:80:6:1800。
5. a kind of preparation method based on hydrogenation of carbon dioxide producing light olefins composite catalyst according to claim 3,
It is characterized in that：In the step S4, in whipping process, first by the circle of stirring 3~5 clockwise after, to stir 3 counterclockwise~
5 circles, untill Ludox and mixed solution are thoroughly mixed.
6. a kind of preparation method based on hydrogenation of carbon dioxide producing light olefins composite catalyst according to claim 3,
It is characterized in that：In the step S6,400~750 DEG C of sintering temperature, roasting time is 1~1.5h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111215080A (en) * | 2018-11-26 | 2020-06-02 | 北京化工大学 | For regulating CO2The hydrogenation target product is C2-4Catalyst for olefin and preparation method thereof |
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| 徐龙伢 等: "CO2加氢制低碳烯烃的Fe/Silicalite-2催化剂研究--I.催化剂性能及反应机理探讨", 《天然气化工》 * |
| 梁兵连等: "二氧化碳加氢合成低碳烯烃的研究进展", 《化工进展》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111215080A (en) * | 2018-11-26 | 2020-06-02 | 北京化工大学 | For regulating CO2The hydrogenation target product is C2-4Catalyst for olefin and preparation method thereof |
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