CN109926052A - A kind of support type patina Quito metal hydroxide catalyst and preparation method thereof - Google Patents
A kind of support type patina Quito metal hydroxide catalyst and preparation method thereof Download PDFInfo
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- CN109926052A CN109926052A CN201910193269.9A CN201910193269A CN109926052A CN 109926052 A CN109926052 A CN 109926052A CN 201910193269 A CN201910193269 A CN 201910193269A CN 109926052 A CN109926052 A CN 109926052A
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Abstract
The invention discloses a kind of support type patina Quito metal hydroxide catalyst and preparation method thereof, the active component of the catalyst is the more metal hydroxides of stratiform, Fe3+With M2+、Me+Laminate main structure is formed, interlayer forms object structure by anion；The carrier of the catalyst is carbon material, molecular sieve, any one or more in inorganic oxide.The present invention is using Fe (II) salt as raw material, it is aoxidized by process, using other stable divalent and polyvalent metal as protective agent, under conditions of more mild, a step is self-assembled into as support type patina Quito metal hydroxide catalyst in synthetic reaction, such catalyst preparation process is simple, structure is extremely stable, adjustable denaturation is strong, the multifunctionality of carrier and catalyst activity component is had both, laminate metal composition and interlayer object anion are adjustable, breach barrier existing for previous patina material, also the construction barriers for being confined to FeOOH catalyst are breached, with extremely wide application value.
Description
Technical field
The invention belongs to PETROLEUM PROCESSINGs, technical field of coal chemical industry, and in particular to one kind is applied to kerosene, and to refine reaction, coal altogether straight
Connect high activity loading type patina Quito metal hydroxide of liquefaction reaction, heavy poor oil lighting reaction and coal tar hydrogenating reaction
Object catalyst and preparation method thereof.
Background technique
In recent years, FeOOH is widely used in DCL/Direct coal liquefaction reaction, heavy poor oil lightweight as catalyst activity component
Change reaction, is mostly derived from FeOOH with cheap cost advantage, and it is living to show ideal reaction in such reaction
Property, therefore DCL/Direct coal liquefaction in recent years, kerosene the industrialized units such as refine altogether and gradually use catalyst based on FeOOH.
FeOOH synthesis process intermediate product is patina, and patina (English name: green rusts) is one kind by divalent ferro element and trivalent
The layered double hydroxide of ferro element composition, belongs to anionic property layered inorganic functional material.By containing Fe (II) and Fe
(III) main layer board of element and interlayer object anion composition.Its unique structural property, so that patina has unique urge
Agent performance, but patina is extremely unstable in an oxygen-containing environment, it is also difficult to it is directly obtained from synthetic reaction, in the lab extremely
Patina material can be just obtained under harsh environment.Patent 200810035857.1 has delivered one kind with FeSO4And Fe2(SO4)3For
Raw material prepares the synthetic method of patina under anaerobic harsh conditions, and not only preparation process is complicated and condition is not easy to control, and with
Aqueous ascorbic acid is synthetic reaction liquid, and cost is considerably higher.
In addition, having numerous research in terms of the modification of FeOOH catalyst in recent years, by adulterating other elements, adjust
The catalytic performance of whole FeOOH catalyst.102380396 A of patent CN has published one kind using coal dust as carrier, with doping
Molybdenum, nickel, tungsten or cobalt γ-FeOOH be the catalyst of active component；104437492 A of patent CN has published a kind of coal dust
As carrier, the FeOOH for adulterating AlOOH is the catalyst of active component.The catalyst that foregoing invention patent is illustrated breaches
There was only catalyst structure of the FeOOH as active component in the past, shows it in respective application response better than pure
Catalyst of the FeOOH as active component, but since other element incorporations are limited, catalyst activity component main structure body
It is still FeOOH, therefore cannot achieve apparent raising on catalyst overall activity.
Summary of the invention
The object of the present invention is to provide a kind of support type patina Quito metal hydroxide catalysts and preparation method thereof.
The technical solution provided by the present invention is: the active component of the catalyst is the more metal hydroxides of stratiform, change
Group becomes [M2+ xFe2+ xOHMe+ 1-xFe3+ 1-xOH](1-x)+(An-)(1-x)/n·mH2O, wherein M2+For Cu2+、Mg2+、Ni2+、Co2+、
Fe2+、Zn2+、Ca2+、Mn2+、Pt2+、Ca2+In any one or more, Me+For Al3+、Cr3+、Co3+、Mo6+、Mn4+、V5+、Ti4+In
Any one or more, An-For Cl-、Br-、NO3 -、ClO3 -、IO3 -、H2PO4 -、OH-、CO3 2-、SO3 2-、SO4 2-、PO4 3-、CrO4 2-、
WO4 2-In any one or more, x is (Fe3++Me+) and (M2++Fe3++Me+) molar ratio, 0.5 < x < 1.0, m is the crystallization water
Amount, m=0~10；Fe3+With M2+、Me+Laminate main structure is formed, interlayer forms object structure by anion；The catalyst
Carrier is any one or more in carbon material, molecular sieve and inorganic oxide.
In catalyst of the present invention, with catalyst gauge, the load capacity of active component is 0.5%~50%, remaining is carrier, is carried
The partial size of body is 1 μm~50000 μm.
Above-mentioned carbon material is the ash of coal dust, semi-coke, active carbon, carbon nanotube, coal gasifying process phosphorus content greater than 40wt.%
At least one of slag；Molecular sieve is Si-Al molecular sieve, catalytic cracking process discards any one in molecular sieve catalyst or two kinds；
Inorganic oxide is silica, aluminium oxide, any one or more in zinc oxide.
Support type patina of the present invention Quito metal hydroxide catalyst the preparation method comprises the following steps: by ferrous salt and M2+It is solvable
Property salt, Me+Soluble-salt it is soluble in water, and carrier is added, is stirred to react 0.5~24 hour, reacted at 20~100 DEG C
It is passed through air or oxygen in Cheng Zhongxiang reaction solution and the pH that precipitating reagent control reaction solution is added is 6~11；It is dehydrated after reaction
And it is dry, obtain support type patina Quito metal hydroxides.
In above-mentioned preparation method, the ferrous salt is ferrous sulfate, ferrous nitrate, frerrous chloride, ferrous bromide, sulfurous acid
More than one in ferrous, iron ammonium sulfate；The M2+Soluble-salt be M2+Sulfate, nitrate or villaumite；The Me+'s
Al in soluble-salt3+、Cr3+And Co3+Soluble-salt be sulfate, nitrate or villaumite, Ti4+And Mo5+Soluble-salt be
Villaumite；The precipitating reagent is NH4HCO3、(NH4)2CO3, urea, ammonium hydroxide, NaHCO3、Na2CO3、K2CO3、KHCO3, sodium acetate, vinegar
Sour potassium, NaOH, KOH, CaCO3、Ca(OH)2In any one or more.
In above-mentioned preparation method, drying temperature is 40~300 DEG C.
The present invention is aoxidized using Fe (II) salt as raw material by process, is protection with other stable divalent and polyvalent metal
Agent, using carbon material, molecular sieve, inorganic oxide as carrier, under conditions of more mild, a step is from group in synthetic reaction
It dresses up as support type patina Quito metal hydroxide catalyst, such catalyst preparation process is simple, structure is extremely stable, can
Modulation is strong, has had both the multifunctionality of carrier and catalyst activity component, and laminate metal composition and interlayer object anion can
It adjusts, breaches barrier existing for previous patina material, also breach the construction barriers for being confined to FeOOH catalyst.The present invention is green
Rust base catalyst can be applied to kerosene and refine reaction, DCL/Direct coal liquefaction reaction, heavy poor oil lighting reaction and coal tar hydrogenating altogether
Reaction has extremely wide application value.
Detailed description of the invention
Fig. 1 is the X-ray diffraction spectrogram of catalyst prepared by embodiment 1.
Fig. 2 is the SEM figure of the patina base catalyst of coal dust load prepared by embodiment 1.
Fig. 3 is the SEM figure of the patina base catalyst of activated alumina load prepared by embodiment 2.
Fig. 4 is the X-ray diffraction spectrogram of catalyst prepared by embodiment 3 and 4.
Fig. 5 is the SEM figure of the patina base catalyst of coal dust load prepared by embodiment 3.
Fig. 6 is the SEM figure of the patina base catalyst of coal dust load prepared by embodiment 4.
Specific embodiment
The present invention will be further described with reference to the accompanying drawings and examples, but protection scope of the present invention is not limited only to this
A little embodiments.
Embodiment 1
With catalyst gauge, the load capacity according to Fe-Co-Mo is 29.6%, by the analytically pure FeCl of 3.96g2·4H2O、
4.76g CoCl2·6H2O、2.73g MoCl5It is dissolved in 100mL deionized water, 10g particle diameter distribution is added into acquired solution is
20~120 μm of pulverized bituminous coal is subsequently passed oxygen and stirs, while the aqueous solution of urea that mass fraction is 5% is added dropwise,
Controlling pH value of solution is 8.8, is reacted 18 hours at 60 DEG C, then filters discharging and the dry 5h at 120 DEG C, obtains coal dust load
Fe (II) Fe (III) patina base catalyst containing Co (II) Mo (IV), X-ray diffraction spectrogram is as shown in Figure 1, in spectrogram
Can be clearly visible the characteristic diffraction peaks of crystal faces such as the more metal hydroxides of stratiform (003), (006), (012), (110) and (113),
The characteristic diffraction peak of the big broad peak of carrier of coal powder near 20 °.Fe (II) Fe (III) containing Co (II) Mo (IV) of coal dust load
Patina base catalyst SEM photograph is as shown in Fig. 2, will become apparent from Fe (II) Fe (III) patina base of hexagonal flake structure in figure
The more metal hydroxides uniform loads of shape are in carrier of coal powder particle surface.
Embodiment 2
With catalyst gauge, the load capacity according to Fe-Ni is 5.0%, will be industrial in 8 cubic metres of commercial synthesis reaction kettle
130 kilograms of FeSO of grade4·7H2O, 120 kg NiSO4·6H2O is dissolved in 5 tons of deionized waters, and 1 is added into acquired solution
Suspension is made in ton active alumina powder, is subsequently passed compressed air and stirs, while volumetric concentration is added by distributor
For 3.7% ammonium hydroxide, controlling pH value of solution is 7.5, is stirred to react at 35 DEG C 6 hours, and subsequent plate compression discharges and at 230 DEG C
Lower drying for 24 hours, obtains Fe (II) Fe (III) patina base catalyst containing Ni (II) of activated alumina load, SEM photograph
As shown in figure 3, the more metal hydroxides of Fe (II) Fe (III) patina base's shape that will become apparent from hexagonal flake structure in figure are uniform
It is carried on active aluminum oxide carrier surface.
Embodiment 3
With catalyst gauge, the load capacity according to Fe-Ni-Zn is 4.0%, will in 8 cubic metres of commercial synthesis reaction kettle
130 kilograms of FeSO of technical grade4·7H2O, 60 kilograms of NiSO4·6H2O, 15 kilograms of ZnSO4·7H2O is dissolved in 5 tons of tap water,
1 ton of active carbon powder is added into acquired solution, suspension is made, is subsequently passed plant instrumentation wind and stirs, be added dropwise simultaneously
The sodium hydrate aqueous solution that mass fraction is 2%, control pH value of solution are 8.0, are reacted 4 hours at 50 DEG C, subsequent plate compression
It discharges and drying for 24 hours, obtains activated carbon supported Fe (II) Fe (III) patina base containing Ni (II) Zn (II) at 200 DEG C
Catalyst.Its X-ray diffraction spectrogram as shown in figure 4, can be clearly visible in spectrogram the more metal hydroxides of stratiform (003),
(006), the characteristic diffraction peak of the crystal faces such as (012), (015), 20 ° nearby the big broad peak of absorbent charcoal carrier and carrier mineral are grey
The characteristic diffraction peak divided.The SEM of activated carbon supported Fe (II) Fe (III) patina base catalyst containing Ni (II) Zn (II) shines
Piece is as shown in figure 5, the more metal hydroxides of Fe (II) Fe (III) patina base's shape that will become apparent from hexagonal flake structure in figure are equal
It is even to be carried on absorbent charcoal carrier surface.
Embodiment 4
With catalyst gauge, the load capacity according to Fe-Mg-Al-Ti is 7.5%, by analytically pure 14.5g (NH4)2Fe
(SO4)2·6H2O、11.84g Mg(NO3)2、15.00g Al(NO3)3·9H2O, 7.59g TiCl4It is dissolved in 250mL deionized water
In, the Yan'an 85g oil plant catalytic cracking process four is added into acquired solution and revolves the discarded molecular sieve catalyst isolated, then
It is passed through air and stirs, while the potassium hydroxide that mass fraction is 1% and the saleratus that mass fraction is 4% is added dropwise
Mixed solution, control pH value of solution are 7.2, are reacted 24 hours at 75 DEG C, then filter discharging and the dry 12h at 120 DEG C, obtain
Fe (II) Fe (III) containing Mg (II) Al (III) Ti (IV) for discarding molecular sieve catalyst load to catalytic cracking process is green
Become rusty base catalyst.Its X-ray diffraction spectrogram as shown in figure 4, can be clearly visible in spectrogram the more metal hydroxides of stratiform (003),
(006), the characteristic diffraction peak of the crystal faces such as (012), (015) is furthermore that catalytic cracking process discards molecular sieve catalytic agent carrier
Characteristic diffraction peak.Catalytic cracking process discards the Fe (II) containing Mg (II) Al (III) Ti (IV) of molecular sieve catalyst load
Fe (III) patina base catalyst SEM photograph is as shown in fig. 6, Fe (II) Fe (III) that will become apparent from hexagonal flake structure in figure is green
The more metal hydroxides uniform loads of base's shape of becoming rusty discard molecular sieve catalyst carrier particle surface in catalytic cracking process.
In order to prove beneficial effects of the present invention, the Mo- for catalyst and the coal dust load that above-described embodiment 1~4 is obtained
FeOOH catalyst (preparation of 102380396 A method of patent CN, wherein metal (Mo-FeOOH) load capacity is 7.5%) is applied to
In the reaction of suspension bed hydro-cracking of vacuum residue, with overweight decompression residuum (525 DEG C of fraction accounting 98wt% of >, sulfur content
4.3wt%) it is used as raw material, reaction condition are as follows: 460 DEG C of reaction temperature；Reaction pressure 22MPa；Catalyst charge 1wt% is (dry
Base ashless coal)；Reaction velocity 0.5kg/ (hL).Obtained heavy oil lighting reaction main result is as shown in table 1.
Table 1
Seen from table 1, catalyst of the present invention shows excellent performance in terms of catalyst activity and desulfurization.
Claims (10)
1. a kind of support type patina Quito metal hydroxide catalyst, it is characterised in that: the active component of the catalyst is layer
The more metal hydroxides of shape, chemical composition are [M2+ xFe2+ xOHMe+ 1-xFe3+ 1-xOH](1-x)+(An-)(1-x)/n·mH2O, wherein M2 +For Cu2+、Mg2+、Ni2+、Co2+、Fe2+、Zn2+、Ca2+、Mn2+、Pt2+、Ca2+In any one or more, Me+For Al3+、Cr3+、
Co3+、Mo6+、Mn4+、V5+、Ti4+In any one or more, An-For Cl-、Br-、NO3 -、ClO3 -、IO3 -、H2PO4 -、OH-、CO3 2-、
SO3 2-、SO4 2-、PO4 3-、CrO4 2-、WO4 2-In any one or more, x is (Fe3++Me+) and (M2++Fe3++Me+) molar ratio,
0.5 < x < 1.0, m are crystallization water, m=0~10；Fe3+With M2+、Me+Laminate main structure is formed, interlayer is made of anion
Object structure；The carrier of the catalyst is any one or more in carbon material, molecular sieve and inorganic oxide.
2. support type patina according to claim 1 Quito metal hydroxide catalyst, it is characterised in that: with catalyst
Meter, the load capacity of active component are 0.5%~50%.
3. support type patina according to claim 1 Quito metal hydroxide catalyst, it is characterised in that: the carbon materials
Material is at least one of the lime-ash of coal dust, semi-coke, active carbon, carbon nanotube, coal gasifying process phosphorus content greater than 40wt.%.
4. support type patina according to claim 1 Quito metal hydroxide catalyst, it is characterised in that: the molecule
Sieve is Si-Al molecular sieve, catalytic cracking process discards any one in molecular sieve catalyst or two kinds.
5. support type patina according to claim 1 Quito metal hydroxide catalyst, it is characterised in that: described inorganic
Oxide is silica, aluminium oxide, any one or more in zinc oxide.
6. being existed according to support type patina Quito metal hydroxide catalyst, feature described in claim 3~5 any one
In: the partial size of the carrier is 1 μm~50000 μm.
7. a kind of preparation method of support type patina described in claim 1 Quito metal hydroxide catalyst, feature exist
In: by ferrous salt and M2+Soluble-salt, Me+Soluble-salt it is soluble in water, and carrier is added, is stirred at 20~100 DEG C
Reaction 0.5~24 hour is passed through air or oxygen into reaction solution and the pH of precipitating reagent control reaction solution is added in reaction process
It is 6~11；It is dehydrated after reaction and dry, obtains support type patina Quito metal hydroxides.
8. the preparation method of support type patina according to claim 7 Quito metal hydroxide catalyst, feature exist
In: the ferrous salt is ferrous sulfate, one in ferrous nitrate, frerrous chloride, ferrous bromide, ferrous sulfite, iron ammonium sulfate
Kind or more；The M2+Soluble-salt be M2+Sulfate, nitrate or villaumite；The Me+Soluble-salt in Al3+、Cr3+
And Co3+Soluble-salt be sulfate, nitrate or villaumite, Ti4+And Mo5+Soluble-salt be villaumite.
9. the preparation method of support type patina according to claim 7 Quito metal hydroxide catalyst, feature exist
In: the precipitating reagent is NH4HCO3、(NH4)2CO3, urea, ammonium hydroxide, NaHCO3、Na2CO3、K2CO3、KHCO3, sodium acetate, acetic acid
Potassium, NaOH, KOH, CaCO3、Ca(OH)2In any one or more.
10. the preparation method of support type patina according to claim 7 Quito metal hydroxide catalyst, feature exist
In: the drying temperature is 40~300 DEG C.
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| CN113457694A (en) * | 2021-06-04 | 2021-10-01 | 华南师范大学 | Composite catalyst and preparation method and application thereof |
| CN114538600A (en) * | 2022-03-28 | 2022-05-27 | 中化学朗正环保科技有限公司 | Iron-carbon coupled microbial film carrier material, reaction device thereof and nitrogen and phosphorus removal system |
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| CN114538600A (en) * | 2022-03-28 | 2022-05-27 | 中化学朗正环保科技有限公司 | Iron-carbon coupled microbial film carrier material, reaction device thereof and nitrogen and phosphorus removal system |
| CN114538600B (en) * | 2022-03-28 | 2023-12-26 | 中化学朗正环保科技有限公司 | Iron-carbon coupled microbial membrane carrier material, reaction device and nitrogen and phosphorus removal system thereof |
| CN115475602A (en) * | 2022-08-29 | 2022-12-16 | 浙江金海高科股份有限公司 | Activated carbon-based adsorption material for carbon-sandwiched cloth and preparation method thereof |
| CN115475602B (en) * | 2022-08-29 | 2023-07-25 | 浙江金海高科股份有限公司 | Activated carbon-based adsorption material for carbon cloth and preparation method thereof |
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