CN107999078A - Solution combustion prepares nickel-base catalyst and its method - Google Patents

Solution combustion prepares nickel-base catalyst and its method Download PDF

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Publication number
CN107999078A
CN107999078A CN201711424120.4A CN201711424120A CN107999078A CN 107999078 A CN107999078 A CN 107999078A CN 201711424120 A CN201711424120 A CN 201711424120A CN 107999078 A CN107999078 A CN 107999078A
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nickel
base catalyst
combustion process
presoma
solution
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CN107999078B (en
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马凤云
武洪丽
莫文龙
张瑞玉
刘景梅
钟梅
唐家维
孙继光
陈隽
高福祥
段春平
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XINJIANG MARKORCHEM Co.,Ltd.
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Xinjiang University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/74Iron group metals
    • B01J23/755Nickel
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08Heat treatment
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/16Reducing
    • B01J37/18Reducing with gases containing free hydrogen
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/17Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by hydrogenation of carbon-to-carbon double or triple bonds
    • C07C29/172Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by hydrogenation of carbon-to-carbon double or triple bonds with the obtention of a fully saturated alcohol
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/52Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Catalysts (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The present invention relates to nickel-base catalyst technical field, is a kind of nickel-base catalyst prepared by solution combustion process and preparation method thereof.The nickel-base catalyst is made by the following method:Weigh a certain amount of six water nickel nitrate or nickel acetate or nickel chloride and nine water aluminum nitrates or aluminum acetate or aluminium chloride, using polypyrrole alkanone as Morphological control agent, deionized water and ethylene glycol mixture, ultrasound are added, presoma test solution is made, by Muffle furnace temperature programming, test solution burns in Muffle furnace, and burner body sample is made, then cool down, grinding, screening, uses H2High temperature reduction, obtains the nickel-base catalyst prepared by solution combustion process.The present invention is a kind of method that is simple, quickly preparing nickel-base catalyst, and catalyst samples produced by the present invention are sheet poromerics, for 1, during 4 butynediols hydrogenation synthesis Isosorbide-5-Nitrae butanediol, have 1, the conversion ratio and selectivity of 4 butynediols are high, the features such as stabilization, are easy to industrialization.

Description

Solution combustion prepares nickel-base catalyst and its method
Technical field
The present invention relates to nickel-base catalyst technical field, is a kind of nickel-base catalyst prepared by solution combustion process Method.
Background technology
For a long time, monopolized always by foreign countries by the catalyst preparation technology of Reppe methods production BDO, it is only a at present Other patent report.China's BDO industries are started in the beginning of this century, are to introduce Reppe from Shanxi three-dimensional group from ISP companies of the U.S. Method production technology starts.It is developed so far, its key technology catalyst fails to realize production domesticization still based on import.
One of document《Journal of Molecular Catalysis》2014.Vo1.28.NO 2.119~125 is by high beautiful Na, Guo Jiangyuan, Zhang Hongxi, Lee " the Ni/SiO that great waves, Xu Yalin, Zhao Yongxiang are delivered2-Al2O3Activity and stabill of the catalyst in water phase hydrogenation system is ground Study carefully " text, the Ni/SiO of different Si contents is prepared for using infusion process2-Al2O3Catalyst.Research shows, when Si contents are 3% When, obtained catalyst samples have preferable Hydrogenation.But use preparation catalyst, in roasting process, meeting Produce substantial amounts of exhaust gas;In the drying process, active component nickel can migrate, and block duct, influence its activity.
The two of document《University Of Shanxi's journal》2010. Vol.33.NO3.413~417 are by Zhang Jianping, Li Haitao, Gao Chun " the Ni/A1 that light, Zhao Yongxiang are delivered2O3The text of the preparation of catalyst and butynediols hydrogenation reaction " one, using incipient impregnation legal system It is 17%Ni/Al for load capacity2O3Catalyst, has investigated the influence of reaction temperature, pressure, time to its catalytic activity.Research Show, be 120 in reaction temperatureoC, 8 MPa of pressure, are hydrogenated with 3 h conditions, prepared catalyst samples are shown preferably Hydrogenation activity.But because temperature is higher, the selectivity of sample reduces, and side reaction enhancing, causes subsequent products separation process to be stranded It is difficult.
Solution combustion method is a kind of quick, simple method for preparing sheet micropore catalysis material.
The content of the invention
The present invention provides a kind of nickel-base catalyst prepared by solution combustion process and its method, overcomes above-mentioned existing The deficiency of technology, it can effectively solve catalyst prepared by existing infusion process, for Isosorbide-5-Nitrae-butynediols hydrogenation synthesis Isosorbide-5-Nitrae- During butanediol, there are active material skewness, Isosorbide-5-Nitrae-butynediols conversion ratio is high, 1,4-butanediol poor selectivity is asked Topic.
One of technical scheme is realized by following measures:It is a kind of to be prepared by solution combustion process Nickel-base catalyst, is made in the steps below:The first step, weighs in a certain amount of six water nickel nitrate or nickel acetate or nickel chloride respectively One kind, and one kind in nine water aluminum nitrates or aluminum acetate or aluminium chloride, using polypyrrole alkanone as Morphological control agent, with volume ratio Example is 1:1 deionized water and ethylene glycol is mixed, and obtains mixed liquor, and ultrasound 20 to 30 minutes, is made presoma test solution, gathers The addition of pyrrolidones is the 0.1% to 0.5% of raw material gross mass, and metallic nickel ions concentration is 0.05 in presoma test solution Mol/L to 1.28 mol/L, aluminium ion concentration are 0.49 mol/L;Second step, presoma test solution is placed in Muffle furnace, from room Warm temperature programming to 400 DEG C to 800 DEG C, burning 6 hours to 8 it is small when, take out, cool down, grind, screening, with 40 mesh to 60 mesh Screening media is sieved, and burner body sample is made;3rd step, burner body sample is placed in fixed bed reactors, at 600 DEG C extremely At a temperature of 900 DEG C, with the H that purity is 99.99%2When reduction burner body sample 4 is small, take out, cool down, grinding, with 80 mesh to 120 Mesh screening media is sieved, and obtains the nickel-base catalyst prepared by solution combustion process.
Here is the further optimization and/or improvements to one of foregoing invention technical solution:
The speed of above procedure heating is 10 DEG C/min to 40 DEG C/min.
The two of technical scheme are realized by following measures:It is a kind of to be prepared by solution combustion process The method of nickel-base catalyst, carries out in the steps below:The first step, weighs a certain amount of six water nickel nitrate or nickel acetate or chlorine respectively Change one kind in nickel, and one kind in nine water aluminum nitrates or aluminum acetate or aluminium chloride, using polypyrrole alkanone as Morphological control agent, with Volume ratio is 1:1 deionized water and ethylene glycol is mixed, and obtains mixed liquor, ultrasound 20 to 30 minutes, is made presoma Test solution, the addition of polypyrrole alkanone are the 0.1% to 0.5% of raw material gross mass, and metallic nickel ions concentration is in presoma test solution 0.05 mol/L to 1.28 mol/L, aluminium ion concentration are 0.49 mol/L;Second step, Muffle furnace is placed in by presoma test solution In, from room temperature temperature programming to 400 DEG C to 800 DEG C, burning 6 hours to 8 it is small when, take out, cool down, grind, screening, with 40 mesh Sieved to 60 mesh screening media, burner body sample is made;3rd step, burner body sample is placed in fixed bed reactors, 600 DEG C at a temperature of 900 DEG C, with the H that purity is 99.99%2When reduction burner body sample 4 is small, take out, cool down, grinding, with 80 mesh Sieved to 120 mesh screening media, obtain the nickel-base catalyst prepared by solution combustion process.
Here is two further optimization and/or improvements to foregoing invention technical solution:
The speed of above procedure heating is 10 DEG C/min to 40 DEG C/min.
The present invention is a kind of method that is simple, quickly preparing nickel-base catalyst, and catalyst samples produced by the present invention are Sheet poromerics, during for Isosorbide-5-Nitrae-butynediols hydrogenation synthesis 1,4-butanediol, have Isosorbide-5-Nitrae-butynediols conversion ratio and Selectivity is high, the features such as stabilization, is easy to industrialization.
Brief description of the drawings
Attached drawing 1 is the nickel-base catalyst burner body sample 1000 times of the present invention by prepared by solution combustion process SEM photograph.
Attached drawing 2 is the nickel-base catalyst burner body sample 50000 of the present invention by prepared by solution combustion process Times SEM photograph.
Embodiment
The present invention from following embodiments limitation, can technique according to the invention scheme and actual conditions determine specifically Embodiment.It is chemicals public in the prior art that chemicals is previously mentioned in the present invention;In the present invention Percentage is mass percent;Room temperature in the present invention refers to 15 DEG C to 25 DEG C of temperature.
With reference to embodiment, the invention will be further described:
Embodiment 1:The nickel-base catalyst prepared by solution combustion process, obtains as follows:The first step, weighs respectively One in one kind in a certain amount of six water nickel nitrate or nickel acetate or nickel chloride, and nine water aluminum nitrates or aluminum acetate or aluminium chloride Kind, it is 1 with volume ratio using polypyrrole alkanone as Morphological control agent:1 deionized water and ethylene glycol is mixed, and is mixed Close liquid, ultrasound 20 to 30 minutes is made presoma test solution, the addition of polypyrrole alkanone for raw material gross mass 0.1% to 0.5%, metallic nickel ions concentration is 0.05 mol/L to 1.28 mol/L in presoma test solution, and aluminium ion concentration is 0.49 mol/ L;Second step, presoma test solution is placed in Muffle furnace, from room temperature temperature programming to 400 DEG C to 800 DEG C, is burnt 6 hours to 8 Hour, take out, cool down, grind, screening, is sieved with 40 mesh to 60 mesh screening media, and burner body sample is made;3rd step, will fire Burn body sample to be placed in fixed bed reactors, at a temperature of 600 DEG C to 900 DEG C, with the H that purity is 99.99%2Reduction burning When body sample 4 is small, take out, cool down, grinding, is sieved with 80 mesh to 120 mesh screening media, obtain preparing by solution combustion process Nickel-base catalyst.
Embodiment 2:The nickel-base catalyst prepared by solution combustion process, obtains as follows:The first step, respectively One kind in a certain amount of six water nickel nitrate or nickel acetate or nickel chloride is weighed, and in nine water aluminum nitrates or aluminum acetate or aluminium chloride One kind, using polypyrrole alkanone as Morphological control agent, with volume ratio be 1:1 deionized water and ethylene glycol is mixed, and is obtained To mixed liquor, ultrasound 20 to 30 minutes is made presoma test solution, the addition of polypyrrole alkanone for raw material gross mass 0.1% or 0.5%, metallic nickel ions concentration is 0.05 mol/L or 1.28 mol/L in presoma test solution, and aluminium ion concentration is 0.49 mol/ L;Second step, presoma test solution is placed in Muffle furnace, from room temperature temperature programming to 400 DEG C or 800 DEG C, burning 6 it is small when or 8 Hour, take out, cool down, grind, screening, is sieved with 40 mesh or 60 mesh screening media, and burner body sample is made;3rd step, will fire Burn body sample to be placed in fixed bed reactors, at a temperature of 600 DEG C or 900 DEG C, with the H that purity is 99.99%2Reduction burning When body sample 4 is small, take out, cool down, grinding, is sieved with 80 mesh or 120 mesh screening media, obtain preparing by solution combustion process Nickel-base catalyst.
Embodiment 3:As the control of above-described embodiment programmed rate, programmed rate is 10 DEG C/min to 40 ℃/min。
Embodiment 4:The nickel-base catalyst prepared by solution combustion process, obtains as follows:The first step, will 20.36 gram of six water nickel nitrate, 36.78 gram of nine water aluminum nitrate and 0.06 gram of polypyrrole alkanone are added to 50 mL deionized waters and second In the mixed solution of glycol(Deionized water and the volume ratio of ethylene glycol are 1:1), ultrasound 30 minutes, is made presoma test solution.The Two steps, temperature programming is carried out by presoma test solution, is risen to 650 DEG C, when constant temperature combustion 8 is small by room temperature, is taken out, cool down, grinds, sieve Point, burner body sample is made.3rd step, by burner body sample at a temperature of 850 DEG C, with the H that purity is 99.99%2Reduction 4 it is small when, obtain the nickel-base catalyst sample 1 prepared by solution combustion process.
Embodiment 5:The nickel-base catalyst prepared by solution combustion process, obtains as follows:The first step, will 20.36 gram of six water nickel nitrate, 36.78 gram of nine water aluminum nitrate and 0.12 gram of polypyrrole alkanone are added to 50 mL deionized waters and second In the mixed liquor of glycol(Deionized water and the volume ratio of ethylene glycol are 1:1), ultrasound 30 minutes, is made presoma sample solution. Second step, presoma sample is placed in Muffle furnace, is risen to 650 DEG C, when constant temperature combustion 8 is small by room temperature, is taken out, cooling, grinds Mill, screening, is made burner body sample;3rd step, by burner body sample at 850 DEG C, with the H that purity is 99.99%2Reduction 4 After hour, the nickel-base catalyst sample 2 prepared by solution combustion process is obtained.
1000 times of SEM of the apparent form of nickel-base catalyst burner body sample made from above-described embodiment 4 and embodiment 5 shine Piece is as shown in Figure 1,50000 times of the apparent form of nickel-base catalyst burner body sample made from above-described embodiment 4 and embodiment 5 SEM photograph is as shown in Figure 2.
Evaluation experimental 1:Sample 1 made from above-described embodiment 4 of 0.60 g is weighed, adds slurry reactor kettle, control is anti- Answer condition:Isosorbide-5-Nitrae-butynediols addition is 30 mL, and reaction temperature is 110 DEG C, H2Pressure is 4 MPa, stir speed (S.S.) 600 R/min, when the reaction time 3 is small, carries out Isosorbide-5-Nitrae-butynediols hydrogenation synthesis 1,4-butanediol reaction.Evaluation result is 1,4- butine Two alcohol conversions reach 99.6%, and the selectivity of 1,4-butanediol reaches 89.3%, and carbonyl value is 1.21mg (KOH)/g.
Evaluation experimental 2:Weigh sample 2 made from above-described embodiment 8 of 0.60 g and add slurry reactor kettle, control reaction Condition:Isosorbide-5-Nitrae-butynediols addition is 30 mL, and reaction temperature is 110 DEG C, H2Pressure is 4 MPa, 600 r/ of stir speed (S.S.) Min, when the reaction time 3 is small, carries out Isosorbide-5-Nitrae-butynediols hydrogenation synthesis 1,4-butanediol reaction.Evaluation result is 1,4- butine two Alcohol conversion reaches 99.8%, and the selectivity of 1,4-butanediol reaches 89.2%, and carbonyl value is 1.17 mg (KOH)/g.
Catalyst samples in one of document, in 150 DEG C of reaction temperature, H2Pressure is 4 MPa, when the reaction time 3 is small Under, its evaluation experimental result reaches 2.9 mg (KOH)/g for carbonyl value.
Catalyst samples in the two of document, in 150 DEG C of reaction temperature, H2Pressure is 4 MPa, when the reaction time 3 is small Under, its evaluation experimental result reaches 4.85 mg (KOH)/g, Isosorbide-5-Nitrae-butynediols conversion ratio 90% for carbonyl value.
According to data above, it can be seen that the nickel-base catalyst prepared by solution combustion process, for Isosorbide-5-Nitrae-butine two When alcohol hydrogenation synthesis 1,4-butanediol is reacted, Isosorbide-5-Nitrae-butynediols high conversion rate, the selectivity of 1,4-butanediol is good, carbonyl value It is low.
In conclusion the present invention is a kind of method that is simple, quickly preparing nickel-base catalyst, catalysis produced by the present invention Agent sample is sheet poromerics, during for Isosorbide-5-Nitrae-butynediols hydrogenation synthesis 1,4-butanediol, has Isosorbide-5-Nitrae-butynediols Conversion ratio and selectivity are high, the features such as stabilization, are easy to industrialization.
Above technical characteristic constitutes the embodiment of the present invention, has stronger adaptability and implementation result, can be according to reality Border needs to increase and decrease non-essential technical characteristic, to meet the needs of different situations.

Claims (4)

1. a kind of nickel-base catalyst prepared by solution combustion process, it is characterised in that obtain in the steps below:The first step, point Also known as take one kind in a certain amount of six water nickel nitrate or nickel acetate or nickel chloride, and nine water aluminum nitrates or aluminum acetate or aluminium chloride In one kind, using polypyrrole alkanone as Morphological control agent, with volume ratio be 1:1 deionized water and ethylene glycol is mixed, Mixed liquor is obtained, presoma test solution is made in ultrasound 20 to 30 minutes, and the addition of polypyrrole alkanone is the 0.1% of raw material gross mass To 0.5%, metallic nickel ions concentration is 0.05 mol/L to 1.28 mol/L in presoma test solution, aluminium ion concentration 0.49 mol/L;Second step, presoma test solution is placed in Muffle furnace, and from room temperature temperature programming to 400 DEG C to 800 DEG C, burning 6 is small When 8 is small, take out, cool down, grind, screening, is sieved with 40 mesh to 60 mesh screening media, and burner body sample is made;3rd step, Burner body sample is placed in fixed bed reactors, at a temperature of 600 DEG C to 900 DEG C, with the H that purity is 99.99%2Reduction When burner body sample 4 is small, take out, cool down, grinding, is sieved with 80 mesh to 120 mesh screening media, obtained by solution combustion process The nickel-base catalyst of preparation.
2. the nickel-base catalyst according to claim 1 or 2 prepared by solution combustion process, it is characterised in that program liter The speed of temperature is 10 DEG C/min to 40 DEG C/min.
3. a kind of method of the nickel-base catalyst according to claim 1 prepared by solution combustion process, its feature exist In carrying out in the steps below:The first step, weighs one kind in a certain amount of six water nickel nitrate or nickel acetate or nickel chloride respectively, and One kind in nine water aluminum nitrates or aluminum acetate or aluminium chloride, is 1 with volume ratio using polypyrrole alkanone as Morphological control agent:1 Deionized water and ethylene glycol are mixed, and obtain mixed liquor, ultrasound 20 to 30 minutes, is made presoma test solution, polypyrrole alkanone Addition be the 0.1% to 0.5% of raw material gross mass, metallic nickel ions concentration is 0.05 mol/L to 1.28 in presoma test solution Mol/L, aluminium ion concentration are 0.49 mol/L;Second step, presoma test solution is placed in Muffle furnace, from room temperature temperature programming to 400 DEG C to 800 DEG C, burning 6 hours to 8 it is small when, take out, cool down, grind, screening, sieved with 40 mesh to 60 mesh screening media, Burner body sample is made;3rd step, burner body sample is placed in fixed bed reactors, at a temperature of 600 DEG C to 900 DEG C, With the H that purity is 99.99%2When reduction burner body sample 4 is small, take out, cool down, grinding, is sieved with 80 mesh to 120 mesh screening media Point, obtain the nickel-base catalyst prepared by solution combustion process.
4. the method for the nickel-base catalyst according to claim 3 prepared by solution combustion process, it is characterised in that journey The speed of sequence heating is 10 DEG C/min to 40 DEG C/min.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109529852A (en) * 2019-01-16 2019-03-29 石河子市中易连疆新能源有限责任公司 Nanoscale Ni-Fe/Al2O3 catalyst and its preparation method and application
CN109772335A (en) * 2019-02-28 2019-05-21 山西潞安矿业(集团)有限责任公司 Nickel-base catalyst and its safe environment protection type solution combustion the preparation method and application

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109529852A (en) * 2019-01-16 2019-03-29 石河子市中易连疆新能源有限责任公司 Nanoscale Ni-Fe/Al2O3 catalyst and its preparation method and application
CN109772335A (en) * 2019-02-28 2019-05-21 山西潞安矿业(集团)有限责任公司 Nickel-base catalyst and its safe environment protection type solution combustion the preparation method and application

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