CN102198958A - Preparation method for high-purity molybdenum trioxide used for hydrofining catalyst of petroleum - Google Patents
Preparation method for high-purity molybdenum trioxide used for hydrofining catalyst of petroleum Download PDFInfo
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- CN102198958A CN102198958A CN2011100836556A CN201110083655A CN102198958A CN 102198958 A CN102198958 A CN 102198958A CN 2011100836556 A CN2011100836556 A CN 2011100836556A CN 201110083655 A CN201110083655 A CN 201110083655A CN 102198958 A CN102198958 A CN 102198958A
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Abstract
The invention relates to a preparation method for high-purity molybdenum trioxide used for a hydrofining catalyst of petroleum, and the method comprises the following steps: carrying out box drying on ammonium tetramolybdate at the temperature of 75-85 DEG C for 18-20 hours, and placing in a sealed packaging bag for 7-10 days; screening dried ammonium tetramolybdate with a 40-mesh screen, and acquiring a screen undersize material; analyzing the contents of molybdenum and impurities in ammonium tetramolybdate used for preparing the high-purity molybdenum trioxide; conveying the treated ammonium tetramolybdate to the furnace end of a rotary tube electric furnace using a screw feeder, and dividing the rotary tube electric furnace into five zones, wherein the temperatures of the five zones are 470+/-5 DEG C, 490+/-5 DEG C, 510+/-5 DEG C, 490+/-5 DEG C, and 470+/-5 DEG C respectively; baking while controlling the rotation speed of the screw feeder at 20-23 Hz and the rotation speed of the rotary tube electric furnace at 30-33 Hz; and screening the product discharged from the furnace, crushing and packaging. The method can be used for improving the solubility (not more than 99.99%) and once yield (not less than 98.5%) of the high-purity molybdenum trioxide, and has the advantages of low production cost and high production efficiency; and the obtained product has the advantages of stable quality and high consistency.
Description
Technical field
The present invention relates to the preparation method of a kind of oil Hydrobon catalyst with high-purity molybdic oxide.
Background technology
Catalyzer is the core of oil refining and petrochemical technology, at the catalyst field catalysts containing molybdenum in occupation of crucial status, oil Hydrobon catalyst particularly has high-purity molybdic oxide (MoO of high dissolubility in need be under specific dipping system, immersion condition
3), its proportion in catalyzer can reach more than 20%, so molybdic oxide (MoO
3) itself and compound thereof be in petrochemical complex and the chemical industry the extremely important and large usage quantity of a class raw material, bringing into play more and more important effect.
Domestic manufacturer this oil Hydrobon catalyst with the production of high dissolubility molybdic oxide be with ammonium molybdate directly at the calcination kiln roasting, mainly have following problem in the production: the one, poorly soluble, insolubles reaches 1.0%; The 2nd, yield rate is about 92%, and all the other 6% enter recovery tower, and 2% is unacceptable product.These two problems are perplexing petroleum chemical enterprise and molybdic oxide (MoO always
3) manufacturing enterprise, affect catalyzer enterprise and molybdic oxide (MoO
3) ordinary production of enterprise, cause production efficiency low, it is more to be worth the waste of very expensive molybdic oxide and catalyzer, and production cost is higher.
Summary of the invention
The problem that the technical problem to be solved in the present invention is solve that existing production technique exists poorly soluble, yield rate is low, the preparation method of a kind of oil Hydrobon catalyst with high-purity molybdic oxide is provided, thereby improves the quality of products, reduce production costs, save the molybdenum resource.
The present invention relates to the preparation method of a kind of oil Hydrobon catalyst with high-purity molybdic oxide, its special character is:
(1) with ammonium tetramolybdate at 75～85 ℃ of box-type drying 18～20h, placed in the airtight package bag 7～10 days then;
(2) drying is left standstill the back ammonium tetramolybdate and cross 40 mesh sieves, extracting screen underflow;
(3) molybdenum and the foreign matter content of the used ammonium tetramolybdate of the high-purity molybdic oxide of analyte preparation;
(4) ammonium tetramolybdate after the processing is sent into return bend electric furnace burner by screw feeder, and the return bend electric furnace is divided into five districts, and five district's temperature are respectively 470 ± 5 ℃, and 490 ± 5 ℃, 510 ± 5 ℃, 490 ± 5 ℃, 470 ± 5 ℃;
(5) controls revolution feeding machine rotating speed is that 20～23Hz, return bend electric furnace rotating speed 30～33Hz carry out roasting;
(6) come out of the stove product through the screening crushing packing.
Above-mentioned oil Hydrobon catalyst is 56～58% with the preparation method of high-purity molybdic oxide, the Mo content of described ammonium tetramolybdate, K content 5～20PPm, W content 50～80PPm, Al ≦ 5, Bi ≦ 5, Ca ≦ 8, Cd ≦ 5, Cu ≦ 3, Fe ≦ 6, Mg ≦ 6, Ni ≦ 3, Na ≦ 10, P ≦ 5, Pb ≦ 5, Sn ≦ 5, Si ≦ 5, Sb ≦ 5, Mn ≦ 3, As ≦ 5.
Above-mentioned oil Hydrobon catalyst is crossed 40 mesh sieves with the preparation method of high-purity molybdic oxide during the product of coming out of the stove screening.
Above-mentioned oil Hydrobon catalyst is with the preparation method of high-purity molybdic oxide, in roasting process stove tail dust material collected and returned return bend electric furnace burner, carries out roasting again, thereby improves yield rate.
The invention provides the preparation method of a kind of oil Hydrobon catalyst with high-purity molybdic oxide, adopt the present invention and compare with high-purity molybdic oxide preparation method with traditional oil Hydrobon catalyst, dried ammonium tetramolybdate is not directly produced, but carry out baked for producing again after dried ammonium tetramolybdate left standstill in the airtight package bag, high-purity molybdic oxide of being produced has following advantage: high-purity molybdic oxide solvability height, solvability 〉=99.99%; Yield rate height 〉=98.5%, constant product quality, high conformity, production cost is low, the production efficiency height.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Embodiment 1
Ammonium tetramolybdate at 75 ℃ of box-type drying 18h, was placed in the airtight package bag 7 days then, drying is left standstill the back ammonium tetramolybdate cross 40 mesh sieves, sampling analysis prepares foreign matter contents such as the Mo of the used ammonium tetramolybdate of high-purity molybdic oxide and K, sees the following form:
| Mo | K | W | |
| Ammonium tetramolybdate | 56.01% | 5ppm | 50ppm |
Sundry item meets MSA-0 trade mark requirement among the GB/T3640-2007, sees the following form the PPm of unit:
| ? | Al | Bi | Ca | Cd | Cu | Fe | Mg | Ni |
| Ammonium tetramolybdate | 5 | 4 | 6 | 5 | 2 | 4 | 6 | 3 |
| ? | Na | P | Pb | Sn | Si | Sb | Mn | As |
| Ammonium tetramolybdate | 8 | 5 | 4 | 5 | 3 | 5 | 1 | 5 |
Ammonium tetramolybdate after handling is sent into return bend electric furnace burner by screw feeder, the return bend electric furnace is divided into five districts, control return bend electric furnace five district's temperature see the following form, control accuracy ± 5 ℃:
| One district | Two districts | Three districts | Four districts | Five districts | |
| Temperature ℃ | 470 | 490 | 510 | 490 | 470 |
Control feeding machine rotating speed is that 20Hz, boiler tube rotating speed 30Hz carry out roasting; Stove tail dust material is returned the collection of burner device automatically and returns return bend electric furnace burner by reclaiming, carry out roasting again; The product of coming out of the stove divides broken through 40 mesh sieves, the extracting screen underflow packing.
The check and analysis product, solvability 99.991%; Yield rate 98.5% satisfies the needs of oil Hydrobon catalyst with high-purity molybdic oxide fully.
Embodiment 2
Ammonium tetramolybdate at 70 ℃ of box-type drying 19h, was placed in the airtight package bag 8 days then, drying is left standstill the back ammonium tetramolybdate cross 40 mesh sieves, sampling analysis prepares foreign matter contents such as the Mo of the used ammonium tetramolybdate of high-purity molybdic oxide and K, sees the following form:
| Mo | K | W | |
| Ammonium tetramolybdate | 56.80% | 12ppm | 57ppm |
Sundry item meets MSA-0 trade mark requirement among the GB/T3640-2007, sees the following form the PPm of unit:
| ? | Al | Bi | Ca | Cd | Cu | Fe | Mg | Ni |
| Ammonium tetramolybdate | 4 | 5 | 8 | 3 | 3 | 6 | 5 | 2 |
| ? | Na | P | Pb | Sn | Si | Sb | Mn | As |
| Ammonium tetramolybdate | 10 | 4 | 5 | 3 | 5 | 4 | 3 | 4 |
Ammonium tetramolybdate after handling is sent into return bend electric furnace burner by screw feeder, the return bend electric furnace is divided into five districts, control return bend electric furnace five district's temperature see the following form, control accuracy ± 5 ℃:
| One district | Two districts | Three districts | Four districts | Five districts | |
| Temperature ℃ | 470 | 490 | 510 | 490 | 470 |
Control feeding machine rotating speed is that 22Hz, boiler tube rotating speed 31Hz carry out roasting; In the roasting process stove tail dust material is returned the collection of burner device automatically and returns return bend electric furnace burner by reclaiming, carry out roasting again; The product of coming out of the stove divides broken through 40 mesh sieves, the extracting screen underflow packing.
The check and analysis product, solvability 99.99%; Yield rate 98.6% satisfies the needs of oil Hydrobon catalyst with high-purity molybdic oxide fully.
Embodiment 3
Ammonium tetramolybdate at 85 ℃ of box-type drying 20h, was placed in the airtight package bag 10 days then, drying is left standstill the back ammonium tetramolybdate cross 40 mesh sieves, sampling analysis prepares foreign matter contents such as the Mo of the used ammonium tetramolybdate of high-purity molybdic oxide and K, sees the following form:
| Mo | K | W | |
| Ammonium tetramolybdate | 58.00% | 20ppm | 80ppm |
Sundry item meets MSA-0 trade mark requirement among the GB/T3640-2007, sees the following form the PPm of unit:
| ? | Al | Bi | Ca | Cd | Cu | Fe | Mg | Ni |
| Ammonium tetramolybdate | 4 | 3 | 6 | 4 | 3 | 5 | 6 | 1 |
| ? | Na | P | Pb | Sn | Si | Sb | Mn | As |
| Ammonium tetramolybdate | 7 | 4 | 3 | 5 | 4 | 2 | 1 | 3 |
Ammonium tetramolybdate after handling is sent into return bend electric furnace burner by screw feeder, and control return bend electric furnace five district's temperature see the following form, control accuracy ± 5 ℃:
| One district | Two districts | Three districts | Four districts | Five districts | |
| Temperature ℃ | 470 | 490 | 510 | 490 | 470 |
Control feeding machine rotating speed is that 23Hz, boiler tube rotating speed 33Hz carry out roasting; Stove tail dust material is returned the collection of burner device automatically and returns return bend electric furnace burner by reclaiming, carry out roasting again; The product of coming out of the stove divides broken through 40 mesh sieves, the screen underflow packing.
The check and analysis product, solvability 99.995%; Yield rate 98.7% satisfies the needs of oil Hydrobon catalyst with high-purity molybdic oxide fully.
Claims (4)
1. an oil Hydrobon catalyst is characterized in that with the preparation method of high-purity molybdic oxide:
(1) with ammonium tetramolybdate at 75～85 ℃ of box-type drying 18～20h, placed in the airtight package bag 7～10 days then;
(2) drying is left standstill the back ammonium tetramolybdate and cross 40 mesh sieves, extracting screen underflow;
(3) molybdenum and the foreign matter content of the used ammonium tetramolybdate of the high-purity molybdic oxide of analyte preparation;
(4) ammonium tetramolybdate after the processing is sent into return bend electric furnace burner by screw feeder, and the return bend electric furnace is divided into five districts, and five district's temperature are respectively 470 ± 5 ℃, and 490 ± 5 ℃, 510 ± 5 ℃, 490 ± 5 ℃, 470 ± 5 ℃;
(5) controls revolution feeding machine rotating speed is that 20～23Hz, return bend electric furnace rotating speed 30～33Hz carry out roasting;
(6) come out of the stove product through the screening crushing packing.
2. oil Hydrobon catalyst according to claim 1 is with the preparation method of high-purity molybdic oxide, and it is characterized in that: the Mo content of described ammonium tetramolybdate is 56～58%, K content 5～20PPm, W content 50～80PPm, Al ≦ 5, Bi ≦ 5, Ca ≦ 8, Cd ≦ 5, Cu ≦ 3, Fe ≦ 6, Mg ≦ 6, Ni ≦ 3, Na ≦ 10, P ≦ 5, Pb ≦ 5, Sn ≦ 5, Si ≦ 5, Sb ≦ 5, Mn ≦ 3, As ≦ 5.
3. oil Hydrobon catalyst according to claim 1 is characterized in that: cross 40 mesh sieves during the product of coming out of the stove screening with the preparation method of high-purity molybdic oxide.
4. oil Hydrobon catalyst according to claim 1 is characterized in that with the preparation method of high-purity molybdic oxide: in roasting process stove tail dust material is collected and returned return bend electric furnace burner, carry out roasting again.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103194624A (en) * | 2013-04-18 | 2013-07-10 | 金堆城钼业股份有限公司 | Method for preparing high-purity molybdenum trioxide |
| CN103663561A (en) * | 2012-09-10 | 2014-03-26 | 中国石油化工股份有限公司 | Recycling method of molybdenum in filament-melting waste acid |
| CN105329945A (en) * | 2015-12-04 | 2016-02-17 | 湖北中澳纳米材料技术有限公司 | Device and method for preparing high-purity and high-dissolvability molybdenum trioxide with industrial molybdic acid |
| CN105819509A (en) * | 2016-03-11 | 2016-08-03 | 金堆城钼业股份有限公司 | Preparation method of pure molybdenum trioxide for catalyst |
| CN111204807A (en) * | 2020-01-15 | 2020-05-29 | 辽宁天桥新材料科技股份有限公司 | Preparation method of high-solubility molybdenum trioxide for nickel-molybdenum-phosphorus petroleum hydrodesulfurization catalyst |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3899284A (en) * | 1973-04-19 | 1975-08-12 | Noranda Mines Ltd | Form of ammonium tetramolybdate and method of preparation |
| CN1826290A (en) * | 2003-07-22 | 2006-08-30 | H.C.施塔克公司 | Method of making MoO2 powders, products made from MoO2 powders, deposition of MoO2 thin films, and methods of using such materials |
| CN101759231A (en) * | 2008-12-24 | 2010-06-30 | 王希全 | Novel roasting process in ammonium molybdate and molybdenum oxide production |
-
2011
- 2011-04-02 CN CN2011100836556A patent/CN102198958A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3899284A (en) * | 1973-04-19 | 1975-08-12 | Noranda Mines Ltd | Form of ammonium tetramolybdate and method of preparation |
| CN1826290A (en) * | 2003-07-22 | 2006-08-30 | H.C.施塔克公司 | Method of making MoO2 powders, products made from MoO2 powders, deposition of MoO2 thin films, and methods of using such materials |
| CN101759231A (en) * | 2008-12-24 | 2010-06-30 | 王希全 | Novel roasting process in ammonium molybdate and molybdenum oxide production |
Non-Patent Citations (1)
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|---|
| 徐志昌等: "四钼酸铵制备过程中的相变研究", 《中国钼业》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103663561A (en) * | 2012-09-10 | 2014-03-26 | 中国石油化工股份有限公司 | Recycling method of molybdenum in filament-melting waste acid |
| CN103194624A (en) * | 2013-04-18 | 2013-07-10 | 金堆城钼业股份有限公司 | Method for preparing high-purity molybdenum trioxide |
| CN105329945A (en) * | 2015-12-04 | 2016-02-17 | 湖北中澳纳米材料技术有限公司 | Device and method for preparing high-purity and high-dissolvability molybdenum trioxide with industrial molybdic acid |
| CN105819509A (en) * | 2016-03-11 | 2016-08-03 | 金堆城钼业股份有限公司 | Preparation method of pure molybdenum trioxide for catalyst |
| CN105819509B (en) * | 2016-03-11 | 2017-09-12 | 金堆城钼业股份有限公司 | A kind of preparation method of the pure molybdenum trioxide of catalyst |
| CN111204807A (en) * | 2020-01-15 | 2020-05-29 | 辽宁天桥新材料科技股份有限公司 | Preparation method of high-solubility molybdenum trioxide for nickel-molybdenum-phosphorus petroleum hydrodesulfurization catalyst |
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Application publication date: 20110928 |