CN104841459A - Preparation method for nickel and cobalt molybdenum tungsten sulfide - Google Patents
Preparation method for nickel and cobalt molybdenum tungsten sulfide Download PDFInfo
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- CN104841459A CN104841459A CN201510268736.1A CN201510268736A CN104841459A CN 104841459 A CN104841459 A CN 104841459A CN 201510268736 A CN201510268736 A CN 201510268736A CN 104841459 A CN104841459 A CN 104841459A
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- nickel
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Abstract
The invention discloses a preparation method for nickel and cobalt molybdenum tungsten sulfide. The preparation method comprises the following steps of preparing cobalt salt or nickel salt or molybdenum salt or tungsten salt solution; adding one of the molybdenum salt solution and the tungsten salt solution or a mixed solution of the molybdenum salt solution and the tungsten salt solution into one of the cobalt salt solution and the nickel salt solution or the mixed solution of the cobalt salt solution and the nickel salt solution, and stirring the mixture for over 30 minutes to obtain composite oxide precipitation of corresponding metals; filtering, washing, drying and sulfurizing the precipitation to obtain cobalt and molybdenum sulfide, nickel and molybdenum sulfide, cobalt and tungsten sulfide, nickel and tungsten sulfide, cobalt and molybdenum tungsten sulfide, nickel and molybdenum tungsten sulfide or nickel and cobalt molybdenum tungsten sulfide. The preparation method disclosed by the invention has the advantages that a precursor before sulfurizing is prepared by a coprecipitation method; the dispersability of the sulfide on a carrier is good; the preparation method is simple and feasible in synthetic process, short in cycle and low in cost.
Description
Technical field
The present invention relates to a kind of preparation method of Hydrobon catalyst, particularly a kind of preparation method preparing presoma by coprecipitation and then obtain nickel cobalt molybdenum tungsten sulfide.
Background technology
In recent years, along with sharply riseing of automobile quantity, the pernicious gas contained in car exhaust gas makes air quality more and more worsen, and countries in the world have put into effect stricter vapour, diesel oil standard in succession.Hydrofining Technology can make distillate high quality, and Hydrobon catalyst is one of link important in Hydrofining Technology.At present, Hydrobon catalyst usually adopts and is incorporated on carrier by dipping by active metal component from solution or suspension, prepares in the method through drying and roasting, and wherein nickel cobalt molybdenum tungsten sulfide is active higher Hydrobon catalyst.
Carry out a large amount of research work probing in Hydrobon catalyst catalytic performance, a viewpoint is universally accepted: the activated centre of sulfide catalyst is positioned at the face, limit of molybdenum sulfide or tungsten sulfide lamella, these lamellas are shorter, face, limit is more, the activity of catalyst is higher, in addition adding the group VIII such as cobalt or nickel metal is the activity that auxiliary agent can improve catalyst effectively, thus the activity that will improve Hydrobon catalyst just need to synthesize high degree of dispersion with group VIII metal be auxiliary agent nanophase molybdenum base or tungsten-based catalyst.Infusion process prepares the common method of loaded catalyst, but it is uneven at carrier surface to there is metal component, and active component particles is large, disperses uneven problem.
CN102166520B discloses a kind of preparation method of Hydrobon catalyst, the method first ammoniacal liquor and polyamines complexing agent is hybridly prepared into double solvents, by the salt containing active component cobalt is added in double solvents, after making salt solubility, add the salt of molybdenum salt or molybdenum salt and other active component or auxiliary agent again, and make it to dissolve, make maceration extract, ageing after impregnated carrier, drying, activation.
CN103007922A discloses a kind of preparation method of Hydrobon catalyst, the method is dissolved in hydrogen peroxide solution by the salt of VIB race metal obtaining maceration extract, with one or more in citric acid, tartaric acid and oxalic acid for dispersant adds in maceration extract, described maceration extract is utilized to flood carrier; Drying, roasting are carried out to impregnation product.
Although carry out dipping when preparing maceration extract improve dispersiveness by adding organic acid or the complexing agent such as ammonia, ethylenediamine, it is very limited to the decentralization improving active component to add these complexing agents, too increases cost; And these complexing agent macromolecule organic acid alkali of calcining removal make sintering temperature relatively high; Ammoniacal liquor is added or organic amine has a large amount of penetrating odors, operating mode extreme difference in the process for preparation of maceration extract; Raw material uses sulfate, nitrate, can discharge sulphur nitrogen oxide pernicious gas during calcining.
Summary of the invention
For the problems referred to above, the object of this invention is to provide a kind of synthesis technique simple, the cycle is short, the method for what cost was low prepare nickel cobalt molybdenum tungsten sulfide.
To achieve these goals, the concrete scheme that the present invention adopts is:
(1) nickel salt, cobalt salt, molybdenum salt and tungsten salt are dissolved in deionized water, are mixed with the settled solution that molar concentration is 0.2 ~ 2.0mol/L respectively;
(2) molybdenum salting liquid is joined in cobalt salt solution or nickel salt solution, Keep agitation 30 minutes, obtain cobalt molybdenum or nickel molybdenum two components precipitate respectively; Tungsten salt solution is joined in cobalt salt solution or nickel salt solution, Keep agitation 30 minutes, obtain cobalt tungsten or nickel tungsten two components precipitate respectively; The mixed solution of molybdenum salt and tungsten salt is joined in cobalt salt solution or nickel salt solution, Keep agitation 30 minutes, respectively obtained cobalt molybdenum tungsten or nickel molybdenum tungsten three components precipitation; The mixed solution of molybdenum salt and tungsten salt is joined in the mixed solution of cobalt salt and nickel salt, Keep agitation 30 minutes, then obtained nickel cobalt molybdenum tungsten Four composition precipitation; By the precipitation obtained through filtering, washing, dry, obtain oxide precursor powder; Or in a kind of or cobalt salt heat-resistant inorganic oxide carrier joined in corresponding cobalt salt solution or nickel salt solution and the mixed solution of nickel salt, stir more than 30 minutes, after adding the mixed solution of a kind of or molybdenum salt and the tungsten salt in molybdenum salting liquid or tungsten salt solution, the composite oxides precipitation of respective metal will be obtained, then filter, wash, dry, obtain oxide precursor powder;
(3) by oxide precursor with containing CS
2decahydronaphthalene solution load high-pressure magnetic stirred tank, wherein CS
2quality be oxide precursor more than 3 times, keep the hydrogen pressure of 2.0-5.0 MPa, be warming up to 200-400 DEG C, insulation 6-24 hour, naturally cool, being taken out by reactant after driving still, take cyclohexane as centrifugal 3 times of washing lotion, vacuum drying 0.5-8.0 hour again, namely obtains the cobalt molybdenum sulphide of non-loading type and support type, nickel molybdenum sulphide, cobalt tungsten sulfide, nickel tungsten sulfide, cobalt molybdenum tungsten sulfide, nickel molybdenum tungsten sulfide and nickel cobalt molybdenum tungsten sulfide.
Described molybdenum salt comprises sodium molybdate or ammonium paramolybdate; Described tungsten salt comprises sodium tungstate or ammonium metatungstate; Described cobalt salt comprises cobalt chloride, cobaltous sulfate or cobalt nitrate; Described nickel salt comprises nickel chloride, nickelous sulfate or nickel nitrate.
Described heat-resistant inorganic oxide carrier is one or more in aluminium oxide, silica, titanium oxide, magnesia, alumina-silica magnesium, silica-alumina, silica-magnesias, silica-titania, silica-zirconia, titania-zirconia, silica-alumina-titania, silicaalumina-magnesia, silica-alumina, zirconia, natural zeolite, synthesis zeolite, non-zeolitic molecular sieves or clay.
Preparation method of the present invention, its outstanding advantages is: the presoma before sulfuration is obtained by coprecipitation, and sulfide is good dispersion on carrier, and synthesis technique is simple, and the cycle is short, and cost is low.
Accompanying drawing explanation
Fig. 1 is the X-ray diffractogram of cobalt tungsten sulfide.
Fig. 2 is the X-ray diffractogram of nickel tungsten sulfide.
Fig. 3 is the X-ray diffractogram of cobalt molybdenum tungsten sulfide.
Fig. 4 is the X-ray diffractogram of nickel molybdenum tungsten sulfide.
Fig. 5 is the X-ray diffractogram of supported cobalt molybdenum sulphide.
Detailed description of the invention
Invention is further illustrated by specific embodiment below in conjunction with accompanying drawing.
Embodiment 1:
Accurately take cobaltous sulfate (CoSO
47H
2o) 12.02g, sodium tungstate (Na
2wO
42H
2o) 4.08g, is dissolved in 50ml distilled water respectively, is made into the solution that concentration is 0.8 and 0.2mol/L, then by Na
2wO
4dropwise is added drop-wise to CoSO
4in solution, stir simultaneously, observe in solution and generate purple precipitation immediately.All solution all drips rear continuation and stirs 0.5h, after reaction terminates, carry out suction filtration, and it is colourless to be washed with distilled water to filtrate, the clean post-drying of washing of precipitate to product.0.6g presoma and 60g are contained 3wt.%CS
2decahydronaphthalene solution load the high-pressure magnetic stirred tank of 100ml, keep the hydrogen pressure of 3.0MPa, be warming up to 350 DEG C, after insulation 6h, naturally cool, after driving still, reactant is taken out, take cyclohexane as centrifugal 3 times of washing lotion, then vacuum drying 2h, namely obtain the sulfide powders of cobalt tungsten.As shown in Figure 1, product is tungsten sulfide and cobalt sulfide, the obvious broadening of diffraction maximum, and intensity is not high, can obtain crystallite dimension at about 12nm according to Scherrer formulae discovery.
Embodiment 2:
Accurately take nickel chloride (NiCl
36H
2o) 9.56g, sodium tungstate (Na
2wO
42H
2o) 4.06g, is dissolved in 50ml distilled water respectively, is made into the solution that concentration is 0.8 and 0.2mol/L, then by Na
2wO
4dropwise drips NiCl
3solution in, stir simultaneously, observe in solution and generate greenish precipitate immediately.All solution all drips rear continuation and stirs half an hour, after reaction terminates, carry out suction filtration, and it is colourless to be washed with distilled water to filtrate, the clean post-drying of washing of precipitate to product.0.6g presoma and 60g are contained 3wt.%CS
2decahydronaphthalene solution load the high-pressure magnetic stirred tank of 100ml, keep the hydrogen pressure of 3.0MPa, be warming up to 350 DEG C, after insulation 6h, naturally cool, after driving still, reactant is taken out, take cyclohexane as centrifugal 3 times of washing lotion, then vacuum drying 2h, namely obtain the sulfide powders of nickel tungsten.As shown in Figure 2, product is tungsten sulfide and nickel sulfide, the obvious broadening of diffraction maximum, and intensity is not high, can obtain crystallite dimension at about 25nm according to Scherrer formulae discovery.
Embodiment 3:
Accurately take cobaltous sulfate (CoSO
47H
2o) 11.2360g, sodium molybdate (Na
2moO
42H
2o) 4.8653g and sodium tungstate (Na
2wO
42H
2o) 6.6270g, is dissolved in 50ml distilled water respectively, is made into the solution that concentration is 0.8,0.4 and 0.4 mol/L respectively, then by Na
2moO
4solution and Na
2wO
4solution mixes, then mixed solution is dropwise added drop-wise to NiCl
3in solution, stir simultaneously, observe in solution and generate purple precipitation immediately.All solution all drips rear continuation stirring 30 minutes, after reaction terminates, carry out suction filtration, and it is colourless to be washed with distilled water to filtrate, the clean post-drying of washing of precipitate to product.0.6g presoma and 60g are contained 3wt.%CS
2decahydronaphthalene solution load the high-pressure magnetic stirred tank of 100ml, keep the hydrogen pressure of 3.0MPa, be warming up to 350 DEG C, after insulation 6h, naturally cool, after driving still, reactant is taken out, take cyclohexane as centrifugal 3 times of washing lotion, then vacuum drying 2h, namely obtain the sulfide powders of cobalt molybdenum tungsten.As shown in Figure 3, product is tungsten sulfide, molybdenum sulfide and cobalt sulfide, the obvious broadening of diffraction maximum, and intensity is not high, can obtain crystallite dimension at about 10nm according to Scherrer formulae discovery.
Embodiment 4:
Accurately take nickel chloride (NiCl
36H
2o) 9.51g, sodium molybdate (Na
2moO
42H
2o) 4.84g and sodium tungstate (Na
2wO
42H
2o) 6.60g, is dissolved in 100ml distilled water respectively, is made into the solution that concentration is 0.4,0.2 and 0.2 mol/L respectively, then by Na
2moO
4solution and Na
2wO
4solution mixes, then mixed solution is dropwise added drop-wise to NiCl
3in solution, stir simultaneously, observe in solution and generate greenish precipitate immediately.All solution all drips rear continuation stirring 30 minutes, after reaction terminates, carry out suction filtration, and it is colourless to be washed with distilled water to filtrate, the clean post-drying of washing of precipitate to product.0.6g presoma and 60g are contained 3wt.%CS
2decahydronaphthalene solution load the high-pressure magnetic stirred tank of 100ml, keep 3.0M to criticize the hydrogen pressure of a, be warming up to 350 DEG C, after insulation 6h, naturally cool, after driving still, reactant is taken out, take cyclohexane as centrifugal 3 times of washing lotion, then vacuum drying 2h, namely obtain the sulfide powders of nickel molybdenum tungsten.As shown in Figure 4, product is tungsten sulfide, molybdenum sulfide and nickel sulfide, the obvious broadening of diffraction maximum, and intensity is not high, can obtain crystallite dimension at about 24nm according to Scherrer formulae discovery.
Embodiment 5:
Accurately take cobaltous sulfate (CoSO
47H
2o) 2.20g, sodium molybdate (Na
2moO
42H
2o) 0.56g, is dissolved in 15ml distilled water respectively, joins in cobalt sulfate solution by activated alumina 2.8g, and Keep agitation 30 minutes, then by Na
2moO
4dropwise is added drop-wise to CoSO
4with in the suspension of aluminium oxide, stir simultaneously, observe in solution and generate lightpink precipitation immediately.All solution all drips rear continuation and stirs 0.5h, after reaction terminates, carry out suction filtration, and it is colourless to be washed with distilled water to filtrate, the clean post-drying of washing of precipitate to product.0.6g presoma and 60g are contained 3wt.%CS
2decahydronaphthalene solution load the high-pressure magnetic stirred tank of 100ml, keep the hydrogen pressure of 3.0MPa, be warming up to 350 DEG C, after insulation 6h, naturally cool, after driving still, reactant is taken out, take cyclohexane as centrifugal 3 times of washing lotion, then vacuum drying 2h, namely obtain the sulfide of supported cobalt molybdenum.As shown in Figure 5, product is the sulfide of alumina support and cobalt molybdenum, the obvious broadening of diffraction maximum, and intensity is not high, can obtain crystallite dimension at about 30nm according to Scherrer formulae discovery.
Above embodiment is only the exemplary description made the present invention; be to be understood that; when not departing from core of the present invention, any simple distortion, amendment or others skilled in the art can not spend the equivalent replacement of creative work all to belong to protection scope of the present invention.
Claims (7)
1. a preparation method for nickel cobalt molybdenum tungsten sulfide, is characterized in that, comprise the following steps:
(1) preparation of solution: be dissolved in deionized water by nickel salt, cobalt salt, molybdenum salt or tungsten salt, is mixed with the settled solution that concentration is 0.2 ~ 2.0mol/L respectively;
(2) preparation of presoma: molybdenum salting liquid is joined in cobalt salt solution or nickel salt solution, Keep agitation 30 minutes, obtains cobalt molybdenum and nickel molybdenum two components precipitate respectively; Tungsten salt solution is joined in cobalt salt solution or nickel salt solution, Keep agitation 30 minutes, obtain cobalt tungsten and nickel tungsten two components precipitate respectively; The mixed solution of molybdenum salt and tungsten salt is joined in cobalt salt solution or nickel salt solution, Keep agitation 30 minutes, cobalt molybdenum tungsten or nickel molybdenum tungsten three components precipitation can be obtained respectively; The mixed solution of molybdenum salt and tungsten salt is joined in the mixed solution of cobalt salt and nickel salt, Keep agitation 30 minutes, then can obtain nickel cobalt molybdenum tungsten Four composition precipitation; By the precipitation obtained through filtering, washing, dry, obtain oxide precursor powder;
(3) preparation of sulfide: by oxide precursor with containing CS
2decahydronaphthalene solution load high-pressure magnetic stirred tank, wherein CS
2quality be oxide precursor more than 3 times, keep the hydrogen pressure of 2.0-5.0 MPa, be warming up to 200-400 DEG C, insulation 6-24 hour, naturally cool, being taken out by reactant after driving still, take cyclohexane as centrifugal 3 times of washing lotion, vacuum drying 0.5-8.0 hour again, namely obtains the sulfide powders of cobalt molybdenum, nickel molybdenum, cobalt tungsten, nickel tungsten, cobalt molybdenum tungsten, nickel molybdenum tungsten, nickel cobalt molybdenum tungsten.
2. the method preparing nickel cobalt molybdenum tungsten sulfide according to claim 1, it is characterized in that in step (2), heat-resistant inorganic oxide carrier being joined in the mixed solution of a kind of or cobalt salt in cobalt salt solution or nickel salt solution and nickel salt, stir more than 30 minutes, after adding the mixed solution of a kind of or molybdenum salt and the tungsten salt in molybdenum salting liquid or tungsten salt solution, the composite oxides precipitation of respective metal will be obtained, after filtration, washing, dry, finally products therefrom is carried out the vulcanizing treatment of step (3), corresponding supported cobalt molybdenum sulphide can be obtained, nickel molybdenum sulphide, cobalt tungsten sulfide, nickel tungsten sulfide, cobalt molybdenum tungsten sulfide, nickel molybdenum tungsten sulfide or nickel cobalt molybdenum tungsten sulfide.
3. the method preparing nickel cobalt molybdenum tungsten sulfide according to claim 1, is characterized in that described molybdenum salt comprises sodium molybdate or ammonium paramolybdate.
4. the method preparing nickel cobalt molybdenum tungsten sulfide according to claim 1, is characterized in that described tungsten salt comprises sodium tungstate or ammonium metatungstate.
5. the method preparing nickel cobalt molybdenum tungsten sulfide according to claim 1, is characterized in that described cobalt salt comprises cobalt chloride, cobaltous sulfate or cobalt nitrate.
6. the method preparing nickel cobalt molybdenum tungsten sulfide according to claim 1, is characterized in that described nickel salt comprises nickel chloride, nickelous sulfate or nickel nitrate.
7. the method preparing nickel cobalt molybdenum tungsten sulfide according to claim 2, is characterized in that described heat-resistant inorganic oxide carrier is one or more in aluminium oxide, silica, titanium oxide, magnesia, alumina-silica magnesium, silica-alumina, silica-magnesias, silica-titania, silica-zirconia, titania-zirconia, silica-alumina-titania, silicaalumina-magnesia, silica-alumina, zirconia, natural zeolite, synthesis zeolite, non-zeolitic molecular sieves or clay.
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| CN106111162A (en) * | 2016-06-17 | 2016-11-16 | 天津大学 | One kind graphene-structured molybdenum sulfide catalyst and preparation method thereof |
| CN106111163A (en) * | 2016-06-17 | 2016-11-16 | 天津大学 | A kind of molybdenum sulfide catalyst of support type high dispersive and preparation method thereof |
| CN106179421A (en) * | 2016-07-19 | 2016-12-07 | 天津大学 | The preparation of sulfide catalyst and the application in lignin conversion thereof |
| CN106238075A (en) * | 2016-07-23 | 2016-12-21 | 天津大学 | Molybdenum sulfide catalyst and preparation thereof and the application in fragrance phenol and ether compound hydrogenation degraded |
| CN107051550A (en) * | 2017-04-24 | 2017-08-18 | 山东大学 | A kind of electro-catalysis water decomposition MoSe2/Co0.85Se composites and preparation method and application |
| CN107790161A (en) * | 2016-08-29 | 2018-03-13 | 中国石油化工股份有限公司 | The method for preparing hydrotreating catalyst |
| CN108144626A (en) * | 2017-11-27 | 2018-06-12 | 南京工业大学 | A kind of lamellar composite type Hydrobon catalyst and preparation method |
| CN115430839A (en) * | 2022-08-25 | 2022-12-06 | 云南电网有限责任公司电力科学研究院 | Preparation method of nickel-molybdenum intermetallic compound and prepared nickel-molybdenum intermetallic compound |
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| CN106111163A (en) * | 2016-06-17 | 2016-11-16 | 天津大学 | A kind of molybdenum sulfide catalyst of support type high dispersive and preparation method thereof |
| CN106111162A (en) * | 2016-06-17 | 2016-11-16 | 天津大学 | One kind graphene-structured molybdenum sulfide catalyst and preparation method thereof |
| CN106111162B (en) * | 2016-06-17 | 2018-12-21 | 天津大学 | One type graphene-structured molybdenum sulfide catalyst and preparation method thereof |
| CN106179421B (en) * | 2016-07-19 | 2019-08-02 | 天津大学 | The preparation of sulfide catalyst and its application in lignin conversion |
| CN106179421A (en) * | 2016-07-19 | 2016-12-07 | 天津大学 | The preparation of sulfide catalyst and the application in lignin conversion thereof |
| CN106238075A (en) * | 2016-07-23 | 2016-12-21 | 天津大学 | Molybdenum sulfide catalyst and preparation thereof and the application in fragrance phenol and ether compound hydrogenation degraded |
| CN107790161B (en) * | 2016-08-29 | 2020-03-17 | 中国石油化工股份有限公司 | Process for preparing hydroprocessing catalysts |
| CN107790161A (en) * | 2016-08-29 | 2018-03-13 | 中国石油化工股份有限公司 | The method for preparing hydrotreating catalyst |
| CN107051550B (en) * | 2017-04-24 | 2019-11-05 | 山东大学 | A kind of electro-catalysis water decomposition MoSe2/Co0.85Se composite material and preparation method and application |
| CN107051550A (en) * | 2017-04-24 | 2017-08-18 | 山东大学 | A kind of electro-catalysis water decomposition MoSe2/Co0.85Se composites and preparation method and application |
| CN108144626A (en) * | 2017-11-27 | 2018-06-12 | 南京工业大学 | A kind of lamellar composite type Hydrobon catalyst and preparation method |
| CN108144626B (en) * | 2017-11-27 | 2021-02-19 | 南京工业大学 | Layered composite hydrodesulfurization catalyst and preparation method thereof |
| CN115430839A (en) * | 2022-08-25 | 2022-12-06 | 云南电网有限责任公司电力科学研究院 | Preparation method of nickel-molybdenum intermetallic compound and prepared nickel-molybdenum intermetallic compound |
| CN115430839B (en) * | 2022-08-25 | 2023-07-07 | 云南电网有限责任公司电力科学研究院 | Preparation method of nickel-molybdenum intermetallic compound and prepared nickel-molybdenum intermetallic compound |
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