CN102897840B - Method for preparing molybdenum trioxide by calcining ammonium dimolybdate - Google Patents
Method for preparing molybdenum trioxide by calcining ammonium dimolybdate Download PDFInfo
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- CN102897840B CN102897840B CN201210451912.1A CN201210451912A CN102897840B CN 102897840 B CN102897840 B CN 102897840B CN 201210451912 A CN201210451912 A CN 201210451912A CN 102897840 B CN102897840 B CN 102897840B
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Abstract
The invention discloses a method for preparing molybdenum trioxide by calcining ammonium dimolybdate. The method comprises the following steps: spreading a ammonium dimolybdate material on a material boat or a conveying belt; driving the ammonium dimolybdate material by the material boat or the conveying belt to pass through a calcination furnace chamber for calcining, wherein air is introduced into the calcination furnace chamber at a flowing speed of 0.10-0.50m/s when calcination is performed; naturally cooling the calcined product to obtain the molybdenum trioxide. According to the method, the temperature zone distribution of the calcination furnace chamber is between 380 DEG C and 468 DEG C; time of the ammonium dimolybdate material passing through the calcination furnace chamber is between 55 minutes and 120 minutes; and the flowing direction of air is opposite to the conveying direction of the ammonium dimolybdate material. The method has the advantages of accurate control in process parameters, low calcination temperature, short calcination time, improved equipment capacity and low processing cost; moreover, the prepared molybdenum trioxide has high activity, can quickly react with phosphoric acid and reaches the requirement of a molybdenum catalyst market on the quality of molybdenum trioxide.
Description
Technical field
The invention belongs to chemical technology field, be specifically related to a kind of method that calcination ammonium dimolybdate prepares molybdic oxide.
Background technology
Along with science and technology is maked rapid progress, market competition is day by day fierce, and molybdenum Application Areas is widened gradually, and market gets more and more to molybdenum Chemicals kind demand, and quality and specification requirement improve day by day.Given this, molybdenum chemical production technical follows era development closely and grows with each passing hour, and develops the product of better quality, develops the demand that short, easy and simple to handle, the reliable and stable product preparation process of flow process meets market.
High reactivity molybdic oxide is new variety of molybdic oxide, be the needs preparing molybdenum series catalyst converting feedstock under the pressure of environmental protection pressure requirement, the molybdenum series catalyst development of adjoint petrochemical complex, coal chemical technology demand simultaneously develops the quality requirements that molybdic oxide proposes.
High reactivity molybdic oxide adopts ammonium molybdate to be raw material, utilizes that ammonium molybdate can be decomposed into ammonia at a certain temperature, steam, molybdic oxide characteristic are prepared.High reactivity molybdic oxide is mainly used in prepares molybdenum series catalyst, and in phosphoric acid solution, have excellent reactive behavior, the molybdenum solution of generation present glassy yellow or yellow-green colour, clarification, without precipitation.
Calcination ammonium molybdate prepares the history that molybdic oxide has many decades, but the molybdic oxide produced is always as the raw material of processing molybdenum powder, and therefore the technique of calcination production of molybdic ammonium molybdic oxide carries out regulation and control around size-grade distribution, crystal morphology, foreign matter content always.High reactivity molybdic oxide is applied in catalyst field, not only there is specific requirement to the impurity of molybdic oxide, size-grade distribution, and also have particular requirement to molybdic oxide response characteristic in the solution, therefore need to prepare to calcination ammonium molybdate the research that molybdic oxide technique carries out in every possible way, and then develop the technique preparing high reactivity molybdic oxide, meet the demand in catalyzer market.
Summary of the invention
Technical problem to be solved by this invention is for above-mentioned the deficiencies in the prior art, provides a kind of calcination ammonium dimolybdate to prepare the method for molybdic oxide.The method process parameter control is accurate, and calcination temperature is low, and the calcination time is short, and equipment capacity improves, and tooling cost is low.The molybdic oxide activity adopting the method to prepare is high, fast with phosphatase reaction speed, and after reaction, solution is glassy yellow or yellow-green colour, clarification, without precipitation, meets the demand of molybdenum series catalyst market to molybdic oxide quality.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of calcination ammonium dimolybdate prepares the method for molybdic oxide, it is characterized in that, the method is: be layed in by ammonium dimolybdate material on material boat or travelling belt, material boat or travelling belt is adopted to drive ammonium dimolybdate material to carry out calcination by calcination stove furnace chamber, calcination passes into air with the flow velocity of 0.10m/s ~ 0.50m/s simultaneously in calcination stove furnace chamber, and after coming out of the stove, naturally cooling obtains molybdic oxide; The warm area of described calcination stove furnace chamber is distributed as 380 DEG C ~ 468 DEG C; Described ammonium dimolybdate material is 55min ~ 120min by the time of calcination stove furnace chamber; The air flow line of described air is contrary with the traffic direction of ammonium dimolybdate material.
Above-mentioned a kind of calcination ammonium dimolybdate prepares the method for molybdic oxide, and the laying amount of described ammonium dimolybdate material is 1.2g/cm
2~ 2.5g/cm
2.
Above-mentioned a kind of calcination ammonium dimolybdate prepares the method for molybdic oxide, and in described calcination stove furnace chamber, air flow quantity is 8m
3/ h ~ 16m
3/ h.
Above-mentioned a kind of calcination ammonium dimolybdate prepares the method for molybdic oxide, and the warm area of described calcination stove furnace chamber is distributed as five warm areas.
Above-mentioned a kind of calcination ammonium dimolybdate prepares the method for molybdic oxide, and the temperature of described five warm areas is followed successively by 380 DEG C, 430 DEG C, 436 DEG C, 468 DEG C and 460 DEG C.
Above-mentioned a kind of calcination ammonium dimolybdate prepares the method for molybdic oxide, and the temperature of described five warm areas is followed successively by 380 DEG C, 380 DEG C, 430 DEG C, 460 DEG C and 460 DEG C.
Above-mentioned a kind of calcination ammonium dimolybdate prepares the method for molybdic oxide, and the length of described calcination stove furnace chamber is 7000mm.
The present invention compared with prior art has the following advantages:
1, method process parameter control of the present invention is accurate, and calcination temperature is low, and the calcination time is short, and equipment capacity improves, and tooling cost is low.
2, the molybdic oxide activity adopting method of the present invention to prepare is high, fast with phosphatase reaction speed, and after reaction, solution is glassy yellow or yellow-green colour, clarification, without precipitation, meets the demand of molybdenum series catalyst market to molybdic oxide quality.
Below in conjunction with drawings and Examples, technical scheme of the present invention is described in further detail.
Accompanying drawing explanation
Fig. 1 is the SEM figure of molybdic oxide prepared by the embodiment of the present invention 1.
Fig. 2 is the XRD figure of molybdic oxide prepared by the embodiment of the present invention 1.
Fig. 3 is the SEM figure of molybdic oxide prepared by the embodiment of the present invention 2.
Fig. 4 is the XRD figure of molybdic oxide prepared by the embodiment of the present invention 2.
Fig. 5 is the SEM figure of molybdic oxide prepared by the embodiment of the present invention 3.
Fig. 6 is the XRD figure of molybdic oxide prepared by the embodiment of the present invention 3.
Fig. 7 is the SEM figure of molybdic oxide prepared by the embodiment of the present invention 4.
Fig. 8 is the XRD figure of molybdic oxide prepared by the embodiment of the present invention 4.
Fig. 9 is the SEM figure of molybdic oxide prepared by the embodiment of the present invention 5.
Figure 10 is the XRD figure of molybdic oxide prepared by the embodiment of the present invention 5.
Figure 11 is the SEM figure of molybdic oxide prepared by the embodiment of the present invention 6.
Figure 12 is the XRD figure of molybdic oxide prepared by the embodiment of the present invention 6.
Embodiment
Embodiment 1
Ammonium dimolybdate material is pressed 1.2g/cm
2be layed on material boat (namely 1.2g ammonium dimolybdate material being laid by every square centimeter of material boat), material boat is adopted to drive ammonium dimolybdate material to carry out calcination by calcination stove furnace chamber, calcination simultaneously passes into the air flow line air contrary with the traffic direction of ammonium dimolybdate material with the flow velocity of 0.15m/s in calcination stove furnace chamber, and to control air flow quantity in calcination stove furnace chamber be 12m
3/ h, after coming out of the stove, naturally cooling obtains molybdic oxide; The warm area of described calcination stove furnace chamber is distributed as five warm areas, and the temperature of five warm areas is followed successively by 380 DEG C, 430 DEG C, 436 DEG C, 468 DEG C and 460 DEG C, and the length of calcination stove furnace chamber is 7000mm; Described ammonium dimolybdate material is 83min by the time of calcination stove furnace chamber.
In molybdic oxide prepared by the present embodiment, the mass percentage of Mo is 66.55%, and this molybdic oxide and phosphoric acid can rapid reactions, the solution clarification of generation, presents yellow-green colour, and without solid residue.
Fig. 1 is the SEM figure of molybdic oxide prepared by the present embodiment, and as can be seen from the figure, molybdenum trioxide particles becomes irregular bulk, and overall dimension is at about 250 μm, and many small-particles are mixed between macrobead; Fig. 2 is the XRD figure of molybdic oxide prepared by the present embodiment, and as can be seen from the figure, diffraction peak position is consistent with molybdic oxide standard diffraction peak position, but diffraction peak intensity is more weak.
Embodiment 2
Ammonium dimolybdate material is pressed 1.4g/cm
2be layed on travelling belt and (namely every square centimeter of travelling belt laid 1.4g ammonium dimolybdate material), travelling belt is adopted to drive ammonium dimolybdate material to carry out calcination by calcination stove furnace chamber, calcination passes into the air flow line air contrary with the traffic direction of ammonium dimolybdate material with the flow velocity of 0.15m/s simultaneously in calcination stove furnace chamber, and to control air flow quantity in calcination stove furnace chamber be 12m3/h, after coming out of the stove, naturally cooling obtains molybdic oxide; The warm area of described calcination stove furnace chamber is distributed as five warm areas, and the temperature of five warm areas is followed successively by 380 DEG C, 430 DEG C, 436 DEG C, 468 DEG C and 460 DEG C, and the length of calcination stove furnace chamber is 7000mm; Described ammonium dimolybdate material is 83min by the time of calcination stove furnace chamber.
In molybdic oxide prepared by the present embodiment, the mass percentage of Mo is 66.55%, and this molybdic oxide and phosphoric acid can rapid reactions, the solution clarification of generation, presents yellow-green colour, and without solid residue.
Fig. 3 is the SEM figure of molybdic oxide prepared by the present embodiment, and as can be seen from the figure, molybdenum trioxide particles becomes irregular bulk, uniform particles, and overall dimension is at about 300 μm, and large particle surface adhering to fine particle; Fig. 4 is the XRD figure of molybdic oxide prepared by the present embodiment, and as can be seen from the figure, diffraction peak position is consistent with molybdic oxide standard diffraction peak position, but diffraction peak intensity is stronger.
Embodiment 3
Ammonium dimolybdate material is pressed 1.2g/cm
2be layed on material boat (namely 1.2g ammonium dimolybdate material being laid by every square centimeter of material boat), material boat is adopted to drive ammonium dimolybdate material to carry out calcination by calcination stove furnace chamber, calcination simultaneously passes into the air flow line air contrary with the traffic direction of ammonium dimolybdate material with the flow velocity of 0.10m/s in calcination stove furnace chamber, and to control air flow quantity in calcination stove furnace chamber be 8m
3/ h, after coming out of the stove, naturally cooling obtains molybdic oxide; The warm area of described calcination stove furnace chamber is distributed as five warm areas, and the temperature of five warm areas is followed successively by 380 DEG C, 380 DEG C, 430 DEG C, 460 DEG C and 460 DEG C, and the length of calcination stove furnace chamber is 7000mm; Described ammonium dimolybdate material is 120min by the time of calcination stove furnace chamber.
In molybdic oxide prepared by the present embodiment, the mass percentage of Mo is 66.56%, and this molybdic oxide and phosphoric acid can rapid reactions, the solution clarification of generation, presents glassy yellow, and without solid residue.
Fig. 5 is the SEM figure of molybdic oxide prepared by the present embodiment, and as can be seen from the figure, molybdenum trioxide particles is sharp-featured bulk, uniform particles, and overall dimension is at about 650 μm, and large particle surface is coarse, does not almost adhere to fine particle; Fig. 6 is the XRD figure of molybdic oxide prepared by the present embodiment, and as can be seen from the figure, diffraction peak position is consistent with molybdic oxide standard diffraction peak position, but diffraction peak intensity is stronger.
Embodiment 4
Ammonium dimolybdate material is pressed 1.4g/cm
2be layed on travelling belt and (namely every square centimeter of travelling belt laid 1.4g ammonium dimolybdate material), travelling belt is adopted to drive ammonium dimolybdate material to carry out calcination by calcination stove furnace chamber, calcination passes into the air flow line air contrary with the traffic direction of ammonium dimolybdate material with the flow velocity of 0.10m/s simultaneously in calcination stove furnace chamber, and to control air flow quantity in calcination stove furnace chamber be 8m3/h, after coming out of the stove, naturally cooling obtains molybdic oxide; The warm area of described calcination stove furnace chamber is distributed as five warm areas, and the temperature of five warm areas is followed successively by 380 DEG C, 380 DEG C, 430 DEG C, 460 DEG C and 460 DEG C, and the length of calcination stove furnace chamber is 7000mm; Described ammonium dimolybdate material is 96min by the time of calcination stove furnace chamber.
In molybdic oxide prepared by the present embodiment, the mass percentage of Mo is 66.55%, and this molybdic oxide and phosphoric acid can rapid reactions, the solution clarification of generation, presents glassy yellow, and without solid residue.
Fig. 7 is the SEM figure of molybdic oxide prepared by the present embodiment, and as can be seen from the figure, molybdenum trioxide particles is sharp-featured bulk, uniform particles, overall dimension is at about 650 μm, and large particle surface is coarse, almost do not adhere to fine particle, basically identical with embodiment 3; Fig. 8 is the XRD figure of molybdic oxide prepared by the present embodiment, and as can be seen from the figure, diffraction peak position is consistent with molybdic oxide standard diffraction peak position, and diffraction peak intensity is embodiment the last 3 comparatively.
Embodiment 5
Ammonium dimolybdate material is pressed 1.4g/cm
2be layed on material boat (namely 1.4g ammonium dimolybdate material being laid by every square centimeter of material boat), material boat is adopted to drive ammonium dimolybdate material to carry out calcination by calcination stove furnace chamber, calcination simultaneously passes into the air flow line air contrary with the traffic direction of ammonium dimolybdate material with the flow velocity of 0.19m/s in calcination stove furnace chamber, and to control air flow quantity in calcination stove furnace chamber be 16m
3/ h, after coming out of the stove, naturally cooling obtains molybdic oxide; The warm area of described calcination stove furnace chamber is distributed as five warm areas, and the temperature of five warm areas is followed successively by 380 DEG C, 430 DEG C, 436 DEG C, 468 DEG C and 460 DEG C, and the length of calcination stove furnace chamber is 7000mm; Described ammonium dimolybdate material is 55min by the time of calcination stove furnace chamber.
In molybdic oxide prepared by the present embodiment, the mass percentage of Mo is 66.62%, and this molybdic oxide and phosphoric acid can rapid reactions, the solution clarification of generation, presents glassy yellow, and without solid residue.
Fig. 9 is the SEM figure of molybdic oxide prepared by the present embodiment, and as can be seen from the figure, molybdenum trioxide particles is sharp-featured bulk, uniform particles, and overall dimension is at about 500 μm, and large particle surface is coarse; Figure 10 is the XRD figure of molybdic oxide prepared by the present embodiment, and as can be seen from the figure, diffraction peak position is consistent with molybdic oxide standard diffraction peak position, and diffraction peak intensity is embodiment the last 5 comparatively.
Embodiment 6
Ammonium dimolybdate material is pressed 2.5g/cm
2be layed on travelling belt and (namely every square centimeter of travelling belt laid 2.5g ammonium dimolybdate material), travelling belt is adopted to drive ammonium dimolybdate material to carry out calcination by calcination stove furnace chamber, calcination passes into the air flow line air contrary with the traffic direction of ammonium dimolybdate material with the flow velocity of 0.50m/s simultaneously in calcination stove furnace chamber, and to control air flow quantity in calcination stove furnace chamber be 16m3/h, after coming out of the stove, naturally cooling obtains molybdic oxide; The warm area of described calcination stove furnace chamber is distributed as five warm areas, and the temperature of five warm areas is followed successively by 380 DEG C, 430 DEG C, 436 DEG C, 468 DEG C and 460 DEG C, and the length of calcination stove furnace chamber is 7000mm; Described ammonium dimolybdate material is 83min by the time of calcination stove furnace chamber.
In molybdic oxide prepared by the present embodiment, the mass percentage of Mo is 66.60%, and this molybdic oxide and phosphoric acid can rapid reactions, the solution clarification of generation, presents glassy yellow, and without solid residue.
Figure 11 is the SEM figure of molybdic oxide prepared by the present embodiment, and as can be seen from the figure, molybdenum trioxide particles is sharp-featured bulk, uniform particles, and overall dimension is at about 500 μm, and large particle surface is coarse; Figure 12 is the XRD figure of molybdic oxide prepared by the present embodiment, and as can be seen from the figure, diffraction peak position is different from embodiment 1 to embodiment 5, and 2 θ angles are occur an obvious diffraction peak near 13 °, and each diffraction peak intensity is the strongest in all embodiments simultaneously.
The element of molybdic oxide prepared by embodiment 1 to embodiment 6 is analyzed, the results are shown in following table:
The results of elemental analyses of the molybdic oxide of table 1 embodiment 1 to embodiment 6 preparation
| Index | Unit | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 |
| Fisher particle size | μm | 13.20 | 13.20 | 13.20 | 13.20 | 13.20 | 13.20 |
| Loose density | g/cm 3 | 1.43 | 1.43 | 1.43 | 1.43 | 1.43 | 1.43 |
| Mo | % | 66.55 | 66.55 | 66.56 | 66.55 | 66.62 | 66.60 |
| Ca | % | 0.0001 | 0.0001 | 0.0001 | 0.0001 | 0.0001 | 0.0001 |
| Mg | % | 0.0001 | 0.0001 | 0.0001 | 0.0001 | 0.0001 | 0.0001 |
| Fe | % | 0.0002 | 0.0002 | 0.0002 | 0.0002 | 0.0002 | 0.0002 |
| K | % | 0.0065 | 0.0065 | 0.0065 | 0.0066 | 0.0065 | 0.0066 |
| Na | % | 0.0006 | 0.0008 | 0.0008 | 0.0006 | 0.0007 | 0.0008 |
| Cu | % | 0.0001 | 0.0001 | 0.0001 | 0.0001 | 0.0001 | 0.0001 |
| Cr | % | 0.0001 | 0.0001 | 0.0001 | 0.0001 | 0.0001 | 0.0001 |
| Ni | % | 0.0002 | 0.0002 | 0.0002 | 0.0002 | 0.0002 | 0.0002 |
As can be seen from Table 1, the molybdic oxide constituent content adopting method calcination of the present invention to prepare is close, and loose density is 1.43g/cm
3, Fisher particle size is 13.2 μm, the basic indifference of constituent content.
The above; it is only preferred embodiment of the present invention; not any restriction is done to the present invention, every above embodiment is done according to invention technical spirit any simple modification, change and equivalent structure change, all still belong in the protection domain of technical solution of the present invention.
Claims (2)
1. a calcination ammonium dimolybdate prepares the method for molybdic oxide, it is characterized in that, the method is: be layed in by ammonium dimolybdate material on material boat or travelling belt, material boat or travelling belt is adopted to drive ammonium dimolybdate material to carry out calcination by calcination stove furnace chamber, calcination passes into air with the flow velocity of 0.10m/s ~ 0.50m/s simultaneously in calcination stove furnace chamber, and after coming out of the stove, naturally cooling obtains molybdic oxide; The warm area of described calcination stove furnace chamber is distributed as 380 DEG C ~ 468 DEG C; Described ammonium dimolybdate material is 55min ~ 120min by the time of calcination stove furnace chamber; The air flow line of described air is contrary with the traffic direction of ammonium dimolybdate material; The laying amount of described ammonium dimolybdate material is 1.2g/cm
2~ 2.5g/cm
2; In described calcination stove furnace chamber, air flow quantity is 8m
3/ h ~ 16m
3/ h; The warm area of described calcination stove furnace chamber is distributed as five warm areas, and the temperature of five warm areas is followed successively by 380 DEG C, 430 DEG C, 436 DEG C, 468 DEG C and 460 DEG C, or is followed successively by 380 DEG C, 380 DEG C, 430 DEG C, 460 DEG C and 460 DEG C.
2. a kind of calcination ammonium dimolybdate according to claim 1 prepares the method for molybdic oxide, it is characterized in that, the length of described calcination stove furnace chamber is 7000mm.
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| CN111204807B (en) * | 2020-01-15 | 2022-09-09 | 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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| CN201302369Y (en) * | 2008-10-06 | 2009-09-02 | 洛阳栾川钼业集团股份有限公司 | Mesh belt type roasting furnace |
| CN101967011A (en) * | 2010-11-01 | 2011-02-09 | 金堆城钼业股份有限公司 | Method for preparing submicron molybdenum trioxide |
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| CN201302369Y (en) * | 2008-10-06 | 2009-09-02 | 洛阳栾川钼业集团股份有限公司 | Mesh belt type roasting furnace |
| CN101967011A (en) * | 2010-11-01 | 2011-02-09 | 金堆城钼业股份有限公司 | Method for preparing submicron molybdenum trioxide |
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