CN106552633A - A kind of preparation method of Ni-based composite catalyst - Google Patents
A kind of preparation method of Ni-based composite catalyst Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 40
- 239000002131 composite material Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 45
- 230000000694 effects Effects 0.000 claims abstract description 6
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 40
- 239000000243 solution Substances 0.000 claims description 30
- 239000000463 material Substances 0.000 claims description 12
- 238000001556 precipitation Methods 0.000 claims description 11
- 238000005984 hydrogenation reaction Methods 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 239000012467 final product Substances 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 6
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 5
- 239000012065 filter cake Substances 0.000 claims description 2
- 239000003643 water by type Substances 0.000 claims description 2
- JLDSOYXADOWAKB-UHFFFAOYSA-N aluminium nitrate Chemical compound [Al+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O JLDSOYXADOWAKB-UHFFFAOYSA-N 0.000 claims 2
- 238000006243 chemical reaction Methods 0.000 abstract description 18
- 238000000034 method Methods 0.000 abstract description 11
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 7
- 238000009903 catalytic hydrogenation reaction Methods 0.000 abstract description 6
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052782 aluminium Inorganic materials 0.000 abstract description 4
- 238000000975 co-precipitation Methods 0.000 abstract description 4
- 239000002904 solvent Substances 0.000 abstract description 2
- 238000013459 approach Methods 0.000 abstract 1
- 230000003197 catalytic effect Effects 0.000 abstract 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 11
- 229910052593 corundum Inorganic materials 0.000 description 11
- 229910001845 yogo sapphire Inorganic materials 0.000 description 11
- 238000013019 agitation Methods 0.000 description 6
- 239000012153 distilled water Substances 0.000 description 5
- 238000006703 hydration reaction Methods 0.000 description 5
- 229910052681 coesite Inorganic materials 0.000 description 4
- 229910052906 cristobalite Inorganic materials 0.000 description 4
- 230000036571 hydration Effects 0.000 description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 229910052682 stishovite Inorganic materials 0.000 description 4
- 229910052905 tridymite Inorganic materials 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 3
- 239000007868 Raney catalyst Substances 0.000 description 3
- 229910000564 Raney nickel Inorganic materials 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 229910020489 SiO3 Inorganic materials 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- DEXFNLNNUZKHNO-UHFFFAOYSA-N 6-[3-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperidin-1-yl]-3-oxopropyl]-3H-1,3-benzoxazol-2-one Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C1CCN(CC1)C(CCC1=CC2=C(NC(O2)=O)C=C1)=O DEXFNLNNUZKHNO-UHFFFAOYSA-N 0.000 description 1
- 229910017121 AlSiO Inorganic materials 0.000 description 1
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 description 1
- 229910020068 MgAl Inorganic materials 0.000 description 1
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical class CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000012018 catalyst precursor Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- -1 magnesium aluminate Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 150000003141 primary amines Chemical class 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Catalysts (AREA)
Abstract
The present invention relates to a kind of method of Ni-based composite catalyst.The method prepares the composite catalyst containing Al, Si, La and Ni by multiple step coprecipitation method.By the ratio for controlling Al, Si, La and Ni element so that catalyst not only has very high resistance to water and activity, and can be according to the intensity for needing change catalyst alkalescence of reaction.Prepared catalyst can be used for having water generating or using water as the catalytic hydrogenation reaction of solvent, and such as in the reaction that the catalytic hydrodeoxygenation to DMF prepares trimethylamine, after 150 DEG C of hydro-thermal process 8h of catalyst, conversion ratio still approaches 100%.
Description
Technical field
The present invention relates to a kind of preparation method of the loaded Ni-based composite catalyst that can be used under hydrothermal conditions, belongs to Catalytic Hydrogenation Techniques neck
Domain.
Technical background
Many industry hydrogenation processes have water generating with water as solvent or in course of reaction so that the catalyst in reaction is chronically at hydro-thermal ring
Border.Therefore, the catalyst used by these hydrogenation processes must have certain resistance to water in hot environment, to ensure the use of catalyst
Efficiency and life-span.In hydrogenation reaction, loaded metalNicatalyst is extensively applied due to cheap, active height.Wherein, especially with oxidation
The metalNicatalyst that aluminium is supported is using extensive.Aluminum oxide is susceptible to hydration in thermal and hydric environment causes catalyst performance to reduce, and limits which and is adding
Use in hydrogen reaction.Therefore, how many documents are for improve Al2O3High temperature resistance to water for the Supported Raney nickel of carrier is carried out
Research.The method of report mainly occupies Al by adding appropriate auxiliary agent2O3Vacancy is suppressing or slow down Al2O3Hydration, urge so as to improve
The resistance to water of agent.Patent application 201410712055.5 reports one kind and uses SiO2Al is improved as auxiliary agent2O3The method of resistance to water, to make
Standby loaded water resistant metal Raney nickel.In addition, by infusion process and kneading method in Al2O3Middle addition rare earth element y b3+、La3+、pr3+、Ce4+、
Sm3+, it is also possible to improve Al2O3Stability under high temperature and vapor existence condition (Acta PhySico-Chimica Sinica, 1996 volume 12, page 971～975).
The oxide for adding alkaline earth Ba, Sr, Ca in aluminum oxide can also improve Al2O3Heat endurance (Applied Catalysis A：General, 1996
Volume 138, page 93～108 of year).Yu Fang etc. has found Fe3+The hydration of aluminum oxide, but effect can also be suppressed not as good as Ni2+、Cu2+、Zr4+Substantially, and
Zn2+、Ce3+、Li+、Mg2+、Co2+The suppression of the hydration of aluminum oxide is become apparent from (petroleum journal, 1999 volume 15, page 25～27).And
Liu Xiyao etc. is then had found in Al2O3After middle introducing MgO, the magnesium aluminate spinel MgAl of generation2O4Make Al2O3Have under hydrothermal conditions preferable
Stability (catalysis journal, 1994 volume 15, page 1～7).In addition, research finds, for some reactions can be changed instead using base catalyst
The selectivity answered.For example, the research such as Zhao Jie finds that base catalyst is conducive to the selectivity of primary amine in the reaction that catalytic hydrogenation of acetonitrile prepares ethamine
(Journal ofCatalysis, 2013 volume 298, page 161～169).
The present patent application is intended preparing Ni/LaAlSiO composite catalysts using multiple step coprecipitation method, improves catalyst stablizing under high temperature hydrothermal condition
Property.Ni/LaAlSiO composite catalysts are prepared using multiple step coprecipitation method and can be prevented effectively from excessive aggregation of the metallic nickel component in catalyst surface, subtracted
Slow metallic Ni particles are grown up.The rare-earth elements La of addition can further occupy Al2O3In room, suppress the hydration under its high temperature thermal and hydric environment,
The resistance to water of catalyst is improved further.Meanwhile, the introducing of La can strengthen the surface alkalinty of catalyst, and the Ni/LaAlSiO for preparing is combined
Catalyst not only has very high hydrothermal energy and catalysis activity, and with appropriate alkalescence, is particularly suited for needing the reaction of surface alkalinty.
The report of the composite catalyst for still not finding W metal is prepared using multiple step coprecipitation method in document.Ask someone in the patent Shen of previous publications
Please in (application number 201410712055.5), Al in Ni/AlSiO catalyst2O3And SiO2The ratio of quality has preferable resistance to water when being 4,
But in the reaction of higher temperature, it is desirable to catalyst has more preferable resistance to water.Therefore step-by-step precipitation method is taken to prepare Ni/LaAlSiO composite catalyzings
Carrier Al in agent, wherein Ni/AlSiO2O3And SiO2Mass ratio be not destroyed, and add metal La can further occupy Al2O3In
Room, suppresses which to be hydrated, and further improves the resistance to water of catalyst.
The Ni/LaAlSiO composite catalysts of the present invention can be used for the reaction of acid amides hydrogenation deoxidation, for example, the catalytic hydrogenation of DMF
Deoxidation prepares the reaction of trimethylamine.Experimental data shows, the ethylene glycol dimethyl ether solution of the DMF for 20%, in 4MPa
Hydrogen Vapor Pressure, at a temperature of 180 DEG C, the catalyst after hydro-thermal process still have very high activity, DMF can be catalyzed
Hydrogenation deoxidation is trimethylamine, and conversion ratio reaches 100%, is selectively 96%.With good industrial prospect.
The content of the invention
Technical scheme is as follows：
A kind of preparation method of Ni/LaAlSiO composite catalysts, it is characterized by：By the Ni (NO of metering3)2·6H2The O and Al (NO for measuring3)3·9H2O
It is dissolved in deionized water together, forms 100mL mixed solution As, by the Na of metering2SiO3·9H2O and the anhydrous Na measured2CO3Be dissolved in from
In sub- water, 100mL mixed solution B are formed.With vigorous stirring, in solution A and B being added drop-wise to 400mL, 80 DEG C of deionized waters simultaneously,
Form the precipitation slip P of celadon；Then by the Ni (NO of metering3)2·6H2O is dissolved in deionized water, forms 100mL mixed solution Cs, will meter
La (the NO of amount3)3·nH2O and the anhydrous Na measured2CO3It is dissolved in deionized water, forms 100mL mixed solution D；With vigorous stirring, will
In the precipitation slip P of the celadon that solution C and D are added drop-wise to above-mentioned 80 DEG C simultaneously, precipitation is formed, by the Washing of Filter Cake being filtrated to get to neutrality,
12h is dried at 120 DEG C, the presoma of Ni/LaAlSiO composite catalysts is obtained final product.The catalyst precursor is for need to be before hydrogenation reaction
Wherein nickel element, with hydrogen reducing, is reduced to the metallic nickel with hydrogenation activity by 400-500 DEG C.
In above-mentioned solution A, the amount of the material containing Ni is 0.05-0.5mol, and the amount of the material containing Al is 0.075-0.75mol.
The Na added in above-mentioned solution B2SiO3·9H2The amount of the material of O be 0.01-0.1mol, anhydrous Na2CO3Material amount be 0.01-0.05
mol。
In above-mentioned solution C, the amount of the material containing Ni is 0.05-0.5mol.
In above-mentioned solution D, the amount of the material containing La is 0.01-0.2mol.
Specific embodiment
With below example and Reference Example, the invention will be further described：
Reference Example 1
Weigh 29.7gNi (NO3)2·6H2O and 23.5gAl (NO3)3·9H2O is dissolved in water, makes 100mL solution；3.8gNaSiO is taken separately3·9H2O
And 21.3gNa2CO3Water is dissolved in, 100mL solution is made.Above-mentioned two parts of solution is added drop-wise to 80 DEG C of 400mL distilled water under agitation simultaneously
In, green precipitate is generated, by the precipitation with distilling after water washing, is dried in 120 DEG C of baking ovens, is obtained final product Al2O3With SiO2Mass ratio is 4
Ni/SiO2-Al2O3The presoma of composite catalyst, sample number into spectrum are Reference Example 1.
Reference Example 2
Weigh 29.7g Ni (NO3)2·6H2O and 7.98g La (NO)3·nH2O is dissolved in water, makes 100mL solution；16.21g Na are taken separately2CO3
Water is dissolved in, 100mL solution is made.Under agitation above-mentioned two parts of solution is added drop-wise in 80 DEG C of 400mL distilled water simultaneously, green is generated heavy
Form sediment, by the precipitation with distilling after water washing, dry in 120 DEG C of baking ovens, obtain final product La (OH)3The Raney nickel presoma for supporting, sample number into spectrum is
Reference Example 2.
Embodiment 1
Weigh 11.9g Ni (NO3)2·6H2O and 9.4g Al (NO3)3·9H2O is dissolved in water, makes 40mL solution；1.5g NaSiO are taken separately3·9H2O and
8.5g Na2CO3Water is dissolved in, 40mL solution is made.Under agitation above-mentioned two parts of solution is added drop-wise in 80 DEG C of 400mL distilled water simultaneously simultaneously
Persistently stir, form celadon slip.17.8g Ni (NO are weighed again3)2·6H2O and 4.8g La (NO3)3·nH2O is dissolved in water, makes 60mL molten
Liquid；9.7g Na are taken separately2CO3Water is dissolved in, 60mL solution is made, under agitation above-mentioned two parts of solution is simultaneously added drop-wise to and above-mentioned to be maintained 80 DEG C
In light green slip and stir, generate green precipitate, by the precipitation with distillation water washing after, dry in 120 DEG C of baking ovens, obtain final product Ni/LaAlSiO
The presoma of composite catalyst, sample number into spectrum are embodiment 1.
Embodiment 2
Weigh 17.8g Ni (NO3)2·6H2O and 14.1gAl (NO3)3·9H2O is dissolved in water, makes 60mL solution；2.3g NaSiO are taken separately3·9H2O
With 12.8g Na2CO3Water is dissolved in, 60mL solution is made.Above-mentioned two parts of solution is added drop-wise to 80 DEG C of 400mL distilled water under agitation simultaneously
In and persistently stir.11.9gNi (NO are weighed again3)2·6H2O and 3.2g La (NO3)3·nH2O is dissolved in water, makes 40mL solution；6.5g is taken separately
Na2CO3Water is dissolved in, 40mL solution is made, under agitation above-mentioned two parts of solution is added drop-wise in upper 80 DEG C of 400mL distilled water and is stirred simultaneously
Mix, generate green precipitate, by the precipitation with distilling after water washing, add 200mL n-butanols, 80 DEG C of water bath methods, then in 120 DEG C of baking ovens
Drying, obtains final product the presoma of Ni/LaAlSiO composite catalysts, and sample number into spectrum is embodiment 2.
Embodiment 3
Prepared catalyst 5g in Reference Example 1,2 and embodiment 1,2 is weighed respectively, is then respectively charged into the hydro-thermal reaction of 40mL water
In kettle, 150 DEG C are warmed up to, keep 8h, then cool to room temperature.Dry at 120 DEG C after filtration, the sample for obtaining is respectively corresponding Reference Example
With sample after the hydro-thermal process of embodiment.
Embodiment 4
The Reference Example 1,2 of phase homogenous quantities is weighed, the Reference Example 1,2 crossed through hydro-thermal process in embodiment 1,2 and embodiment 3, embodiment 1,2
Sample, is loaded in fixed bed reactors respectively, is warmed up to 450 DEG C, is passed through hydrogen, and then hydrogen flowing quantity 100mL/min, reductase 12 h will
Temperature of reactor is set in 180 DEG C, and system pressure brings up to 4MPa, is passed through containing 20wt%N, and the glycol dimethyl ether of dinethylformamide is molten
Liquid, mass space velocity are 1h-1, reaction result is shown in Table 1,2.
Table 1, hydro-thermal process procatalyst conversion ratio and selectivity to DMF catalytic hydrogenation
| Catalyst | Conversion ratio | It is selective |
| Reference Example 1 | 99% | 92% |
| Reference Example 2 | 19% | 96% |
| Embodiment 1 | 98% | 97% |
| Embodiment 2 | 100% | 97% |
Table 2, hydro-thermal process rear catalyst conversion ratio and selectivity to DMF catalytic hydrogenation
| Catalyst | Conversion ratio | It is selective |
| Reference Example 1 | 53% | 90% |
| Reference Example 2 | 5% | 91% |
| Embodiment 1 | 95% | 94% |
| Embodiment 2 | 100% | 96% |
Claims (6)
1. a kind of preparation method of Ni/LaAlSiO composite catalysts, it is characterized by：By the Ni (NO of metering3)2·6H2O and metering
Al(NO3)3·9H2O is dissolved in deionized water together, forms 100mL mixed solution As, by the Na of metering2SiO3.9H2O is anhydrous with metering
Na2CO3It is dissolved in deionized water, forms 100mL mixed solution B.With vigorous stirring, by solution A and B be added drop-wise to simultaneously 400mL,
In 80 DEG C of deionized waters, the precipitation slip P of celadon is formed；Then by the Ni (NO of metering3)2·6H2O is dissolved in deionized water, forms 100mL
Mixed solution C, by the La (NO of metering3)3.nH2O and the anhydrous Na measured2CO3It is dissolved in deionized water, forms 100mL mixed solution D；
With vigorous stirring, in the precipitation slip P of the celadon for solution C and D being added drop-wise to above-mentioned 80 DEG C simultaneously, precipitation is formed, by what is be filtrated to get
Washing of Filter Cake is dried 12h at 120 DEG C to neutrality, obtains final product the presoma of Ni/LaAlSiO composite catalysts.
2., according to claim 1, the presoma of described Ni/LaAlSiO composite catalysts need to be at 400-500 DEG C with hydrogen before for hydrogenation reaction
Wherein nickel element is reduced to the metallic nickel with hydrogenation activity by reduction.
3., according to claim 1, in described solution A, the amount of the material containing Ni is 0.05-0.5mol, and the amount of the material containing Al is
0.075-0.75mol。
4. according to claim 1, the Na added in described solution B2SiO3.9H2The amount of the material of O be 0.01-0.1mol, anhydrous Na2C03
Material amount be 0.01-0.05mol.
5., according to claim 1, in described solution C, the amount of the material containing Ni is 0.05-0.5mol.
6., according to claim 1, in described solution D, the amount of the material containing La is 0.01-0.2mol.
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Cited By (2)
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| CN112675865A (en) * | 2021-01-06 | 2021-04-20 | 中国地质大学（武汉） | High-activity and high-stability supported nickel catalyst and preparation method and application thereof |
| CN114749191A (en) * | 2022-03-24 | 2022-07-15 | 淮阴工学院 | Ni/P-attapulgite clay catalyst and preparation method and application thereof |
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| CN112675865A (en) * | 2021-01-06 | 2021-04-20 | 中国地质大学（武汉） | High-activity and high-stability supported nickel catalyst and preparation method and application thereof |
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| CN114749191A (en) * | 2022-03-24 | 2022-07-15 | 淮阴工学院 | Ni/P-attapulgite clay catalyst and preparation method and application thereof |
| CN114749191B (en) * | 2022-03-24 | 2023-06-30 | 淮阴工学院 | Ni/P-attapulgite clay catalyst and preparation method and application thereof |
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