CN102909038A - Preparation process of catalyst containing tungsten nickel molybdenum fluoride components - Google Patents
Preparation process of catalyst containing tungsten nickel molybdenum fluoride components Download PDFInfo
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- CN102909038A CN102909038A CN2012104126620A CN201210412662A CN102909038A CN 102909038 A CN102909038 A CN 102909038A CN 2012104126620 A CN2012104126620 A CN 2012104126620A CN 201210412662 A CN201210412662 A CN 201210412662A CN 102909038 A CN102909038 A CN 102909038A
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- nickel molybdenum
- catalyst
- tungsten nickel
- maceration extract
- components
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Abstract
The invention relates to a preparation process of a catalyst containing tungsten nickel molybdenum fluoride components. The preparation process is characterized by including firstly, preparing impregnation liquid A containing fluoride components, preparing impregnation liquid B containing tungsten nickel molybdenum components; quickly mixing and uniformly stirring the impregnation liquid A and the impregnation liquid B prepared, placing the mixture into a vacuum rotary impregnator within 30 minutes to sufficiently mix with catalyst carrier with a certain outer diameter and shape, completing saturated impregnation; then activating the impregnated catalyst carrier at high temperature to obtain a catalyst containing the tungsten nickel molybdenum fluoride components. Since the impregnation liquid A containing the fluoride components and the impregnation liquid B containing the tungsten nickel molybdenum components are prepared separatately and saturated impregnation of the catalyst carrier is completed within 30 minutes after the two impregnation liquids are mixed, precipitation after the impregnation liquid A containing the fluoride components and the impregnation liquid B containing the tungsten nickel molybdenum components contact with each other for a long time is avoided, original two procedures of impregnating, drying and roasting can be reduced into one, and production efficiency is improved.
Description
Technical field
The present invention relates to a kind of catalyst preparation process of tungsten nickel molybdenum fluorine component, the catalyst preparation process of the tungsten nickel molybdenum fluorine component that particularly a kind of production procedure is short, efficient is high.
Background technology
The catalyst of tungstenic nickel molybdenum fluorine component in process of production, need to be fluorine-containing at carrier dipping, the maceration extract of tungsten, molybdenum, nickel component, because fluorine-containing solution is with the solution mixed preparing maceration extract of tungstenic, molybdenum, nickel component the time, can chemical reaction occur slowly generate yellow acicular crystal thing, thereby thereby can't once prepare maceration extract and once finish dipping process, therefore at present traditional process route is: preparation fluorine maceration extract, tungsten nickel molybdenum maceration extract--carrier and fluorine maceration extract dipping--drying and roasting--carrier and tungsten nickel molybdenum maceration extract flood--drying and roasting.Need at twice dipping, drying and roasting, operation is many, and production efficiency is low, and cost is high.
Summary of the invention
The technical problem to be solved in the present invention provides the catalyst preparation process of the tungsten nickel molybdenum fluorine component that a kind of production procedure is short, efficient is high.
For solving the problems of the technologies described above, technical scheme of the present invention is: a kind of catalyst preparation process of tungsten nickel molybdenum fluorine component, and its innovative point is that described processing step is: at first prepare the maceration extract A of fluorine component, preparation is the maceration extract B of tungstenic nickel molybdenum component simultaneously; After the maceration extract A for preparing and maceration extract B mixed rapidly and stirring, within 30 minutes, put into the vacuum rotating impregnator, finish saturated dipping with the catalyst carrier that is placed in one; Then the catalyst carrier behind the dipping is carried out high-temperature activation and make the catalyst that contains tungsten nickel molybdenum fluorine component.
Further, after described maceration extract A and maceration extract B mix rapidly and stir, within 20 minutes, put into the vacuum rotating impregnator.
The invention has the advantages that: the maceration extract B of the maceration extract A of fluorine component and tungstenic nickel molybdenum component is preparation separately, and in after mixing 30 minutes catalyst carrier is finished saturated dipping, avoid the maceration extract A of fluorine component and the maceration extract B Long contact time of tungstenic nickel molybdenum component precipitation to occur, original twice dipping, drying process can be reduced to together, on the basis that guarantees product quality, the integral production cycle shortened to 23 hours from 35 hours, enhanced productivity.
The specific embodiment
At first prepare maceration extract A: ammonium fluoride is mixed with the aqueous solution of certain content, makes the maceration extract A of fluorine component; The concentration of ammonium fluoride is 70-300g/l.
Preparation maceration extract B: with a certain amount of nickel nitrate, ammonium metatungstate, the dissolving of ammonium molybdate water, be mixed with by a certain percentage maceration extract B; Wherein, the concentration of ammonium metatungstate is 200-800g/l, nickel nitrate 30-300g/l, ammonium molybdate 50-500g/l.
Dipping: after maceration extract A and maceration extract B mixed rapidly and stirring, within 30 minutes, put into the vacuum rotating impregnator, fully mix with the catalyst carrier with certain external diameter, shape that is placed in one in advance, carry out saturated dipping.
The length of resting period was on the impact of catalyst quality after maceration extract A mixed with maceration extract B:
Give an example one: feeding intake with amount theory on the active component is respectively F content 3%, WO
3Content 18%, NiO content 1.0%, M
0O
3The catalyst soakage of content 5% is example:
Mixed rear 10 minutes, amount is respectively on the metal when flooding: F 2.96%, WO
317.89%, NiO 1.0%, M
0O
34.94%, all to meet in theory water gaging flat for the content of each metal component in the catalyst, and amount fully on the activity component impregnation.
Mixed rear 20 minutes, amount is respectively on the metal when flooding: F 2.96%, WO
317.86%, NiO 0.98%, M
0O
34.92%, all to meet in theory water gaging flat for the content of each metal component in the catalyst, and amount fully on the activity component impregnation.
Mixed rear 30 minutes, amount is respectively on the metal when flooding: F 2.94%, WO
317.84%, NiO 0.98%, M
0O
34.94%, all to meet in theory water gaging flat for the content of each metal component in the catalyst, and amount fully on the activity component impregnation.
Mixed rear 40 minutes, amount is respectively on the metal when flooding: F 2.94%, WO
317.64%, NiO 0.85%, M
0O
34.75%, the content decrease of each metal component is obvious in the catalyst, and amount is insufficient on the activity component impregnation.
Mixed rear 50 minutes, amount is respectively on the metal when flooding: F 2.94%, WO
316.20%, NiO 0.66%, M
0O
34.05%, significantly descending appears in the content of each metal component in the catalyst, and amount is extremely insufficient on the activity component impregnation.
Give an example two: feeding intake with amount theory on the active component is respectively F content 4%, WO
3Content 27%, NiO content 3.0%, M
0O
3The catalyst soakage of content 16% is example:
Mixed rear 10 minutes, amount is respectively on the metal when flooding: F 4.01%, WO
326.90%, NiO 2.96%, M
0O
315.94%, all to meet in theory water gaging flat for the content of each metal component in the catalyst, and amount fully on the activity component impregnation.
Mixed rear 20 minutes, amount is respectively on the metal when flooding: F 3.98%, WO
326.88%, NiO 2.93%, M
0O
315.90%, all to meet in theory water gaging flat for the content of each metal component in the catalyst, and amount fully on the activity component impregnation.
Mixed rear 30 minutes, amount is respectively on the metal when flooding: F 3.98%, WO
326.80%, NiO 2.90%, M
0O
315.80%, all to meet in theory water gaging flat for the content of each metal component in the catalyst, and amount fully on the activity component impregnation.
Mixed rear 40 minutes, amount is respectively on the metal when flooding: F 3.94%, WO
325.06%, NiO 2.35%, M
0O
314.75%, obviously descending appears in the content of each metal component in the catalyst, and amount is insufficient on the activity component impregnation.
Mixed rear 50 minutes, amount is respectively on the metal when flooding: F 3.96%, WO
323.42%, NiO 1.88%, M
0O
314.03%, significantly descending appears in the content of each metal component in the catalyst, and amount is extremely insufficient on the activity component impregnation.
Sum up conclusion: no matter be the maceration extract of high concentration or low concentration, mix rear 30 minutes with interior dipping, amount is fully stable on the reactive metal, and effect is better, and best dip time is within 20 minutes.
Final drying roasting: at last the catalyst carrier behind the dipping is carried out high-temperature activation and make the catalyst that contains tungsten nickel molybdenum fluorine component.
Claims (2)
1. the catalyst preparation process of a tungsten nickel molybdenum fluorine component is characterized in that described processing step is: at first prepare the maceration extract A of fluorine component, the maceration extract B of preparation while tungstenic nickel molybdenum component; After the maceration extract A for preparing and maceration extract B mixed rapidly and stirring, within 30 minutes, put into the vacuum rotating impregnator, finish saturated dipping with the catalyst carrier that is placed in one; Then the catalyst carrier behind the dipping is carried out high-temperature activation and make the catalyst that contains tungsten nickel molybdenum fluorine component.
2. the catalyst preparation process of tungsten nickel molybdenum fluorine component according to claim 1 is characterized in that: after described maceration extract A and maceration extract B mix rapidly and stir, put into the vacuum rotating impregnator within 20 minutes.
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|---|---|---|---|
| CN2012104126620A CN102909038A (en) | 2012-10-25 | 2012-10-25 | Preparation process of catalyst containing tungsten nickel molybdenum fluoride components |
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|---|---|---|---|
| CN2012104126620A CN102909038A (en) | 2012-10-25 | 2012-10-25 | Preparation process of catalyst containing tungsten nickel molybdenum fluoride components |
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| CN102909038A true CN102909038A (en) | 2013-02-06 |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4285836A (en) * | 1979-09-04 | 1981-08-25 | Gulf Research & Development Company | Impregnating solution for hydrotreating catalyst manufacture and production thereof |
| US4328128A (en) * | 1979-09-04 | 1982-05-04 | Gulf Research & Development Company | Hydrotreating catalyst and manufacture thereof |
| CN1360009A (en) * | 2000-12-18 | 2002-07-24 | 中国石化集团齐鲁石油化工公司 | Catalyst for hydromodifying poor middle distillate oil and its preparing process |
| CN1887420A (en) * | 2006-07-26 | 2007-01-03 | 中国石油大庆石化公司研究院 | Petroleum wax hydrofining catalyst and its prepn process |
| JP3872612B2 (en) * | 1998-03-20 | 2007-01-24 | 中国石油化工集団公司 | Catalysts containing molybdenum and / or tungsten for the hydrotreatment of light oil distillates and their preparation |
| CN101089132A (en) * | 2006-06-16 | 2007-12-19 | 中国石油化工股份有限公司 | Fraction oil hydrodesulfurizing catalyst and its prepn process |
| CN101270300A (en) * | 2008-04-30 | 2008-09-24 | 中国石油天然气股份有限公司 | A hydrodeoxygenation catalyst for biodiesel production |
-
2012
- 2012-10-25 CN CN2012104126620A patent/CN102909038A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4285836A (en) * | 1979-09-04 | 1981-08-25 | Gulf Research & Development Company | Impregnating solution for hydrotreating catalyst manufacture and production thereof |
| US4328128A (en) * | 1979-09-04 | 1982-05-04 | Gulf Research & Development Company | Hydrotreating catalyst and manufacture thereof |
| JP3872612B2 (en) * | 1998-03-20 | 2007-01-24 | 中国石油化工集団公司 | Catalysts containing molybdenum and / or tungsten for the hydrotreatment of light oil distillates and their preparation |
| CN1360009A (en) * | 2000-12-18 | 2002-07-24 | 中国石化集团齐鲁石油化工公司 | Catalyst for hydromodifying poor middle distillate oil and its preparing process |
| CN101089132A (en) * | 2006-06-16 | 2007-12-19 | 中国石油化工股份有限公司 | Fraction oil hydrodesulfurizing catalyst and its prepn process |
| CN1887420A (en) * | 2006-07-26 | 2007-01-03 | 中国石油大庆石化公司研究院 | Petroleum wax hydrofining catalyst and its prepn process |
| CN101270300A (en) * | 2008-04-30 | 2008-09-24 | 中国石油天然气股份有限公司 | A hydrodeoxygenation catalyst for biodiesel production |
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Application publication date: 20130206 |