CN106824188A - A kind of preparation of tungsten-based catalyst of carrying transition metal and application process - Google Patents
A kind of preparation of tungsten-based catalyst of carrying transition metal and application process Download PDFInfo
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- CN106824188A CN106824188A CN201710020782.9A CN201710020782A CN106824188A CN 106824188 A CN106824188 A CN 106824188A CN 201710020782 A CN201710020782 A CN 201710020782A CN 106824188 A CN106824188 A CN 106824188A
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- tungsten
- transition metal
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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
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/56—Platinum group metals
- B01J23/64—Platinum group metals with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/652—Chromium, molybdenum or tungsten
- B01J23/6527—Tungsten
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
Abstract
Preparation and application process the present invention relates to a kind of tungsten-based catalyst of carrying transition metal, the method is：Tungsten-based catalyst is prepared using low temperature liquid phase hydrothermal synthesis method, one or more transition metal is directly loaded in into carrier surface using sodium borohydride chemical reduction method is obtained support type tungsten-based catalyst；This tungsten-based catalyst is well mixed with cellulose and water, and hydrogenation catalyst degraded prepares ethylene glycol in being enclosed within autoclave；Cellulose can efficiently, high selectivity, be catalytically conveted to ethylene glycol in high yield, ethylene glycol yield is up to 76.3%.Present invention process is simple, favorable reproducibility, and raw materials are inorganic compound, and the reaction raw materials of its application direction are renewable resource, and reaction condition is gentle, and cellulose conversion ratio and ethylene glycol yield are high；Ethylene glycol is important industrial chemicals.
Description
Technical field
A kind of tungsten-based catalyst the present invention relates to carrying transition metal is prepared and its application on cellulose, especially
The New Tungsten base supported catalyst degraded cellulose constituted using tungstic acid and iridium, rhodium, platinum, palladium, ruthenium even load component,
High selectivity changes into ethylene glycol.
Background technology
Today's society, the mankind are continuously increased to the demand of the energy, but the non-renewable fossil combustion such as traditional oil, coal
Material faces worsening shortages, and the consumption of fossil fuel causes that ecological degeneration and environmental problem become more acute, therefore
Find efficient, free of contamination reproducible biomass resource extremely urgent.Cellulose is the maximum renewable money of yield on the earth
Source, source is enriched very much, such as wood waste of stalk, production of forestry in agricultural production etc. is very cheap using cost.
Ethylene glycol is important energy liquid fuel, is also very important polyester synthesis raw material, can serve as glassine paper, fiber, skin
Leather, the wetting agent of adhesive, it is also possible to as antifreezing agent, plasticizer, surfactant etc., are former widely used organic chemical industries
Material.
It is considered as a kind of very promising problem that cellulose degradation prepares ethylene glycol, but a large amount of due to existing in cellulose
Intramolecular and intermolecular hydrogen bond action so that the structure of cellulose is highly stable, and conventional people are merely able to by fiber
Element first carries out sour water solution, and recycling obtains glucose carries out the trans-utilization in later stage, and this process is not only cumbersome, and produces tight
The problem of environmental pollution (US 4476331) of weight.Chinese patent (A of CN 101648140) with water as solvent, using W2C/Al2O3、
W2C/AC、Ni-W2The catalyst such as C/AC in 120-300 DEG C of catalytic hydrogenation degraded cellulose 30min, by single step reaction process reality
Existing cellulose Efficient Conversion is ethylene glycol, but catalyst preparation process is complicated, is not suitable for amplifying production.(Green in document
The 3075-3083 of Chemistry 17 (2015)) microcrystalline cellulose is extracted from timber, by Ru/W/AC, Ru/AC+H2WO4Etc. urging
Agent degraded cellulose, but ethylene glycol yield is relatively low.Chinese patent (A of CN 101723802) describes cellulose and uses transition
Metallic iron, cobalt, nickel, ruthenium, rhodium, palladium, iridium, platinum and molybdenum, the metallic state of tungsten, carbide, nitride, phosphide are catalytic active component
The multimetal reforming catalyst of composition carries out hydrogenolysis and prepares ethylene glycol in 120-300 DEG C, 1-12MPa and 1-3h, and the method needs consumption
More hydrogen source and energy, and ethylene glycol yield only 60% or so.Therefore need to find efficiently, the catalyst of energy-saving and environmental protection drop
Solution cellulose, prepares the ethylene glycol of high yield.
Chinese patent (A of CN 103030179) discloses one kind with dust technology and sodium tungstate as raw material, under the conditions of being easier to
The method of Hydrothermal Synthesiss tungstic trioxide nano-slice, the method does not need the pre-treatment of high temperature, calcining etc, and synthesis temperature is relatively low,
So as to reduce energy consumption and reaction cost, it is easy to batch production.From the point of view of being consulted on document, not yet there is transition metal direct so far
It is supported on catalytic hydrogenation degraded cellulose on tungstic trioxide nano-slice so that cellulose is converted completely, and is prepared with this
The ethylene glycol of high yield.
The content of the invention
Technical problem：Object of the present invention is to provide a kind of tungsten-based catalyst of carrying transition metal preparation and should
With method, the catalyst has reactivity higher, can prepare the ethylene glycol of high yield to cellulose catalytic hydrogenation, is fine
The plain conversion of dimension is with effective using there is provided important approach.
Technical scheme：The present invention is preparation and the application process of a kind of tungsten-based catalyst of carrying transition metal, the preparation
Method includes：Catalyst carrier is to mix generation wolframic acid by dilute nitric acid solution and sodium tungstate solution to precipitate, then through hydro-thermal
Tungstic trioxide nano-slice prepared by synthetic method, catalyst activity component is made up of transition metal, using sodium borohydride electronation
The reducing metal ions of transition metal are supported on tungstic trioxide nano-slice surface by method into atom, are prepared into carrying transition metal
Tungsten-based catalyst.
Wherein：
The tungsten-based catalyst of described carrying transition metal is loaded catalyst, and transition metal is iridium, rhodium, platinum, palladium, ruthenium
In one or more.
The reducing metal ions of transition metal are supported on three oxygen by described utilization sodium borohydride chemical reduction method into atom
Change tungsten nanometer sheet surface, be the tungsten-based catalyst by carrying transition metal with tungstic trioxide nano-slice as major catalyst, uniformly
Dispersion is that reducing agent passes through magnetic agitation by transition metal iridium, rhodium, platinum, palladium, ruthenium using sodium borohydride in aqueous
Kind or various Direct Uniforms be supported on tungstic trioxide nano-slice.
The carrier-borne transition metal granular size be 2~6nm, on the basis of the weight of catalyst, iridium, rhodium, platinum, palladium,
The weight of ruthenium load is the 0.5%-30% of tungsten base load body weight.
The application of tungsten-based catalyst of carrying transition metal prepared by the method for the present invention is：The catalyst is applied to fibre
That ties up plain high selectivity changes into ethylene glycol.
Wherein：
The cellulose high selectivity changes into ethylene glycol, is be well mixed cellulose, tungsten-based catalyst and water, and
Hydrogenation catalyst degraded prepares ethylene glycol in being enclosed within autoclave.
Cellulose high selectivity changes into ethylene glycol, wherein, cellulose is 50 with the mass ratio of tungsten-based catalyst:1-5:
1, cellulose quality is 1 with water volume ratio:10-1:50 answer temperature for 150-300 DEG C, and the reaction time is 0.5-4h, reacts H2Pressure
Power is 0.5-8MPa.
Cellulose high selectivity changes into ethylene glycol, and preferred reaction temperature is 200-250 DEG C, at room temperature in reactor
H2Preferred initial pressure 3-6MPa, preferred reaction time is 1-3h.
Beneficial effect：The present invention compared with prior art, with advantages below：
1. with cellulose as raw material, raw material sources extensively, while economic crisis can be alleviated, reduce petrochemical industry to the present invention
The consumption of raw material, the protection for ecological environment has great importance.
2. it is catalyst that the present invention uses direct support type tungstic acid, and synthesis condition is gentle, low production cost, and adds
Hydrogen catalysis efficiency high, cellulose conversion can reach 100%, and the yield of ethylene glycol is higher than 70%.
3. the product liquid component that in the present invention prepared by hydrogenation catalyst cellulose is less, and composition is more single, predominantly second two
Alcohol, is important chemical industry and medicine intermediate.
The catalyst that the method is used is cheap, environmental protection, it is easy to mass produce；Reaction condition is gentle, and cellulose turns
Change and the yield of ethylene glycol is high；The ethylene glycol of high yield is important industrial chemicals.
Specific embodiment
Technical solution of the present invention is described in further detail below by embodiment.
Embodiment 1
WO3The preparation of catalyst：The concentrated nitric acid that 7ml concentration is 65% is diluted to the dust technology that concentration is 10% first
40mL；Then 2g Disodium tungstate (Na2WO4) dihydrates are dissolved in during 20mL distilled water adds dilute nitric acid solution, are loaded after magnetic agitation 30min
In the water heating kettle of polytetrafluoroethylene (PTFE), 180 DEG C of reaction 3h；Room temperature is finally cooled to, is repeatedly washed with ethanol and distilled water, 80 DEG C true
Sky dries 6h, and the catalyst for obtaining is tungstic trioxide nano-slice, is expressed as WO3。
Embodiment 2
Ru/WO3The preparation of catalyst：First by 1g WO3It is dissolved in 25mL distilled water, ultrasonic 10min；Then stirred in magnetic force
5mL ruthenium trichlorides standard liquid (0.41g/100mL) are added under the conditions of mixing；Finally repeatedly washed with ethanol and distilled water, 80 DEG C of vacuum
12h is dried, the catalyst 1wt.% containing ruthenium for obtaining is expressed as 1%Ru/WO3。
Other conditions are constant, only change and add ruthenium trichloride standard liquid amount, can obtain tungstic acid of the different component containing ruthenium
Catalyst, respectively 0.5%Ru/WO3, 1%Ru/WO3, 2%Ru/WO3, 3%Ru/WO3, 10%Ru/WO3, 30%Ru/WO3。
Embodiment 3
Ir/WO3、Rh/WO3、Pt/WO3、Pd/WO3The preparation of catalyst：Preparation process and embodiment 2 are close, and difference is
Ruthenium trichloride is changed into iridous chloride, chlorine rhodium acid sodium, hexachloro sodium platinate, chlorine palladium acid sodium respectively before preparing.Ir in catalyst,
The mass content of Rh, Pt, Pd is 1wt.%, and 1%Ir/WO is designated as respectively3, 1%Rh/WO3, 1%Pt/WO3, 1%Pd/WO3。
Embodiment 4
Different tungsten-based catalyst hydrocracking fibrin reactions：The water for weighing 1g celluloses, 0.25g catalyst and 40ml adds
Enter in autoclave, reactor is tightened into sealing.The nitrogen of 2MPa is passed through, is vented, removed in reactor in triplicate
Air.The hydrogen of 4MPa is then passed to, mixing speed is 1000 rpms, is warming up to 240 DEG C and keeps temperature 2h.Reaction
Room temperature is cooled to after end, product liquid, solid residue is collected.The catalyst for using is respectively in table 1：(1) 0.5%Ru/
WO3, (2) 1%Ru/WO3, (3) 2%Ru/WO3, (4) 3%Ru/WO3, (5) 10%Ru/WO3, (6) 30%Ru/WO3, (7) 1%
Ir/WO3, (8) 1%Rh/WO3, (9) 1%Pt/WO3, (10) 1%Pd/WO3.Ethylene glycol yield is analyzed with GC.
The different tungsten-based catalyst catalytic hydrogenation cellulose Performance comparisions of table 1
As can be seen from the table, conversion ratio and second of the tungsten-based catalyst of metallic element ruthenium (1wt.%) load to cellulose
The yield highest of glycol, shows more excellent catalysis activity.
Embodiment 5
Ru/WO at a temperature of differential responses3The comparing of cellulose catalytic conversion performance, is shown in Table 2 on (1wt.%) catalyst.Remove
Catalyst is different with reaction temperature outer, and reaction condition is with embodiment 4.
Ru/WO at a temperature of the differential responses of table 23The comparing of cellulose catalytic conversion performance on catalyst
Embodiment 6
Ru/WO under the differential responses time3The comparing of cellulose catalytic conversion performance, is shown in Table 3 on (1wt.%) catalyst.Remove
Catalyst is different with the reaction time outer, and reaction condition is with embodiment 4.
Ru/WO under the differential responses time of table 33The comparing of cellulose catalytic conversion performance on catalyst
Embodiment 7
Ru/WO under different hydrogen pressure3The comparing of cellulose catalytic conversion performance, is shown in Table 4 on (1wt.%) catalyst.Remove
Catalyst is different with Hydrogen Vapor Pressure outer, and reaction condition is with embodiment 4.
Ru/WO under the different hydrogen pressure of table 43The comparing of cellulose catalytic conversion performance on catalyst
Claims (8)
1. a kind of preparation method of the tungsten-based catalyst of carrying transition metal, it is characterised in that：The preparation method includes：Catalyst
Carrier is to mix generation wolframic acid by dilute nitric acid solution and sodium tungstate solution to precipitate, three oxygen for then being prepared through hydrothermal synthesis method
Change tungsten nanometer sheet, catalyst activity component is made up of transition metal, using sodium borohydride chemical reduction method by the gold of transition metal
Category ion reduction is supported on tungstic trioxide nano-slice surface into atom, is prepared into the tungsten-based catalyst of carrying transition metal.
2. according to a kind of carrying transition metal described in claim 1 tungsten-based catalyst preparation method, it is characterised in that：Institute
The tungsten-based catalyst of the carrying transition metal stated be loaded catalyst, transition metal be iridium, rhodium, platinum, palladium, ruthenium in one kind or
It is various.
3. according to a kind of carrying transition metal described in claim 1 tungsten-based catalyst preparation method, it is characterised in that：Institute
The reducing metal ions of transition metal are supported on tungstic trioxide nano-slice by the utilization sodium borohydride chemical reduction method stated into atom
Surface, be the tungsten-based catalyst by carrying transition metal with tungstic trioxide nano-slice as major catalyst, be uniformly dispersed in water-soluble
It is by magnetic agitation that one or more in transition metal iridium, rhodium, platinum, palladium, ruthenium is straight reducing agent using sodium borohydride in liquid
Connect and be uniformly supported on tungstic trioxide nano-slice.
4. according to a kind of carrying transition metal described in claim 1 tungsten-based catalyst preparation method, it is characterised in that：Institute
Carrier-borne transition metal granular size is stated for 2~6nm, on the basis of the weight of catalyst, iridium, rhodium, platinum, palladium, the weight of ruthenium load
Amount is the 0.5%-30% of tungsten base load body weight.
5. a kind of application of the tungsten-based catalyst of carrying transition metal prepared by the method for claim 1, its feature exists
In：Ethylene glycol is changed into by what the catalyst was applied to cellulose high selectivity.
6. according to the carrying transition metal described in claim 5 tungsten-based catalyst application, it is characterised in that：The cellulose
High selectivity changes into ethylene glycol, is to be well mixed cellulose, tungsten-based catalyst and water, and be enclosed within autoclave
Hydrogenation catalyst degraded prepares ethylene glycol.
7. according to the carrying transition metal described in claim 5 tungsten-based catalyst application, it is characterised in that：Cellulose Gao Xuan
Selecting property changes into ethylene glycol, wherein, cellulose is 50 with the mass ratio of tungsten-based catalyst:1-5:1, cellulose quality and water body
Product is than being 1:10-1:50 answer temperature for 150-300 DEG C, and the reaction time is 0.5-4h, reacts H2Pressure is 0.5-8MPa.
8. according to the carrying transition metal described in claim 7 tungsten-based catalyst application, it is characterised in that：Cellulose Gao Xuan
Selecting property changes into ethylene glycol, and preferred reaction temperature is 200-250 DEG C, at room temperature H in reactor2Preferred initial pressure 3-
6MPa, preferred reaction time is 1-3h.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106910900A (en) * | 2017-02-28 | 2017-06-30 | 上海电力学院 | A kind of Pd base fuel battery catalyst of APTMS functionalization and preparation method and application |
| CN109608496A (en) * | 2018-12-27 | 2019-04-12 | 武汉工程大学 | A kind of environment-friendly preparation method thereof of fosfomycin phenylethylamine calt |
| CN111266109A (en) * | 2018-12-04 | 2020-06-12 | 中国科学院上海硅酸盐研究所 | Ru-WOxNanowire HER catalyst and preparation method thereof |
| CN112002913A (en) * | 2020-08-20 | 2020-11-27 | 常州大学 | Oxygen-enriched vacancy tungsten oxide supported catalyst and preparation method thereof |
| CN112206773A (en) * | 2020-11-08 | 2021-01-12 | 河南理工大学 | Catalyst for preparing ethanol from cellulose and preparation method and application thereof |
| CN112570012A (en) * | 2019-09-27 | 2021-03-30 | 中国石油化工股份有限公司 | Catalyst for preparing bio-based ethylene glycol and preparation method and application thereof |
| CN112760677A (en) * | 2020-12-28 | 2021-05-07 | 中国科学技术大学 | Iridium-tungsten alloy nano material, preparation method thereof and application of iridium-tungsten alloy nano material as acidic oxygen evolution reaction electrocatalyst |
| CN114849694A (en) * | 2022-06-07 | 2022-08-05 | 西北工业大学 | Catalyst based on metal-loaded tungsten oxide hydrogenated nitroarene and preparation method and application thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106910900A (en) * | 2017-02-28 | 2017-06-30 | 上海电力学院 | A kind of Pd base fuel battery catalyst of APTMS functionalization and preparation method and application |
| CN111266109A (en) * | 2018-12-04 | 2020-06-12 | 中国科学院上海硅酸盐研究所 | Ru-WOxNanowire HER catalyst and preparation method thereof |
| CN109608496A (en) * | 2018-12-27 | 2019-04-12 | 武汉工程大学 | A kind of environment-friendly preparation method thereof of fosfomycin phenylethylamine calt |
| CN112570012A (en) * | 2019-09-27 | 2021-03-30 | 中国石油化工股份有限公司 | Catalyst for preparing bio-based ethylene glycol and preparation method and application thereof |
| CN112570012B (en) * | 2019-09-27 | 2022-10-11 | 中国石油化工股份有限公司 | Catalyst for preparing bio-based ethylene glycol and preparation method and application thereof |
| CN112002913A (en) * | 2020-08-20 | 2020-11-27 | 常州大学 | Oxygen-enriched vacancy tungsten oxide supported catalyst and preparation method thereof |
| CN112206773A (en) * | 2020-11-08 | 2021-01-12 | 河南理工大学 | Catalyst for preparing ethanol from cellulose and preparation method and application thereof |
| CN112760677A (en) * | 2020-12-28 | 2021-05-07 | 中国科学技术大学 | Iridium-tungsten alloy nano material, preparation method thereof and application of iridium-tungsten alloy nano material as acidic oxygen evolution reaction electrocatalyst |
| CN112760677B (en) * | 2020-12-28 | 2021-12-10 | 中国科学技术大学 | Iridium-tungsten alloy nano material, preparation method thereof and application of iridium-tungsten alloy nano material as acidic oxygen evolution reaction electrocatalyst |
| CN114849694A (en) * | 2022-06-07 | 2022-08-05 | 西北工业大学 | Catalyst based on metal-loaded tungsten oxide hydrogenated nitroarene and preparation method and application thereof |
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