CN102897840A - 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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- CN102897840A CN102897840A CN2012104519121A CN201210451912A CN102897840A CN 102897840 A CN102897840 A CN 102897840A CN 2012104519121 A CN2012104519121 A CN 2012104519121A CN 201210451912 A CN201210451912 A CN 201210451912A CN 102897840 A CN102897840 A CN 102897840A
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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 the method that a kind of 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 the molybdenum Application Areas is widened gradually, and market is more and more to molybdenum Chemicals kind demand, and quality and specification requirement improve day by day.Given this, the 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.
The high reactivity molybdic oxide is new variety of molybdic oxide, be to prepare the needs that the molybdenum series catalyst raw material changes under the pressure of the environmental protection pressure requirement, the quality requirements of following simultaneously the molybdenum series catalyst development of petrochemical complex, coal chemical technology demand that molybdic oxide is proposed develops.
The high reactivity molybdic oxide is that to adopt ammonium molybdate be raw material, utilizes ammonium molybdate can be decomposed at a certain temperature ammonia, steam, molybdic oxide characteristic and is prepared.The high reactivity molybdic oxide is mainly used in the preparation molybdenum series catalyst, and has good reactive behavior in phosphoric acid solution, and the molybdenum solution of generation presents glassy yellow or yellow-green colour, clarification, without precipitation.
The calcination ammonium molybdate prepares the history of the existing many decades of molybdic oxide, but the molybdic oxide of producing is always as the raw material of processing molybdenum powder, so the technique of calcination production of molybdic ammonium molybdic oxide is carried out regulation and control around size-grade distribution, crystal morphology, foreign matter content always.The high reactivity molybdic oxide is applied in catalyst field, not only impurity, the size-grade distribution of molybdic oxide there is specific requirement, and the response characteristic of molybdic oxide in solution also there is particular requirement, therefore need to prepare molybdic oxide technique to the calcination ammonium molybdate and carry out in every possible way research, and then develop the technique for preparing the high reactivity molybdic oxide, satisfy 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 the calcination temperature is low, and the calcination time is short, and equipment capacity improves, and tooling cost is low.Adopt the molybdic oxide activity of the method preparation high, fast with phosphatase reaction speed, after the reaction solution be glassy yellow or yellow-green colour, clarification, without precipitation, satisfy molybdenum series catalyst market to the demand of 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: the ammonium dimolybdate material is layed on material boat or the travelling belt, adopt material boat or travelling belt to drive the ammonium dimolybdate material and 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, the rear naturally cooling of coming out of the stove obtains molybdic oxide; The warm area of described calcination stove furnace chamber is distributed as 380 ℃～468 ℃; Described ammonium dimolybdate material is 55min～120min by the time of calcination stove furnace chamber; The air flow line of described air is opposite 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 air flow quantity is 8m in the described calcination stove furnace chamber
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 ℃, 430 ℃, 436 ℃, 468 ℃ and 460 ℃.
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 ℃, 380 ℃, 430 ℃, 460 ℃ and 460 ℃.
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 the calcination temperature is low, and the calcination time is short, and equipment capacity improves, and tooling cost is low.
2, adopt the molybdic oxide activity of method preparation of the present invention high, fast with phosphatase reaction speed, after the reaction solution be glassy yellow or yellow-green colour, clarification, without precipitation, satisfy molybdenum series catalyst market to the demand of molybdic oxide quality.
Below in conjunction with drawings and Examples, technical scheme of the present invention is described in further detail.
Description of drawings
Fig. 1 is the SEM figure of the molybdic oxide of the embodiment of the invention 1 preparation.
Fig. 2 is the XRD figure of the molybdic oxide of the embodiment of the invention 1 preparation.
Fig. 3 is the SEM figure of the molybdic oxide of the embodiment of the invention 2 preparations.
Fig. 4 is the XRD figure of the molybdic oxide of the embodiment of the invention 2 preparations.
Fig. 5 is the SEM figure of the molybdic oxide of the embodiment of the invention 3 preparations.
Fig. 6 is the XRD figure of the molybdic oxide of the embodiment of the invention 3 preparations.
Fig. 7 is the SEM figure of the molybdic oxide of the embodiment of the invention 4 preparations.
Fig. 8 is the XRD figure of the molybdic oxide of the embodiment of the invention 4 preparations.
Fig. 9 is the SEM figure of the molybdic oxide of the embodiment of the invention 5 preparations.
Figure 10 is the XRD figure of the molybdic oxide of the embodiment of the invention 5 preparations.
Figure 11 is the SEM figure of the molybdic oxide of the embodiment of the invention 6 preparations.
Figure 12 is the XRD figure of the molybdic oxide of the embodiment of the invention 6 preparations.
Embodiment
Embodiment 1
The ammonium dimolybdate material is pressed 1.2g/cm
2Be layed in (being to lay 1.2g ammonium dimolybdate material on every square centimeter of material boat) on the material boat, adopt the material boat to drive the ammonium dimolybdate material and carry out calcination by calcination stove furnace chamber, calcination passes into the air flow line air opposite with the traffic direction of ammonium dimolybdate material with the flow velocity of 0.15m/s simultaneously in calcination stove furnace chamber, and air flow quantity is 12m in the control calcination stove furnace chamber
3/ h, the rear naturally cooling of coming out of the stove 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 ℃, 430 ℃, 436 ℃, 468 ℃ and 460 ℃, and the length of calcination stove furnace chamber is 7000mm; Described ammonium dimolybdate material is 83min by the time of calcination stove furnace chamber.
The quality percentage composition of Mo is 66.55% in the molybdic oxide of the present embodiment preparation, and this molybdic oxide and phosphoric acid can rapid reactions, and the solution of generation is clarified, presented yellow-green colour, and without solid residue.
Fig. 1 is the SEM figure of the molybdic oxide of the present embodiment preparation, and as can be seen from the figure, the molybdic oxide particle becomes irregular bulk, and overall dimension is about 250 μ m, and many small-particles are mixed between the macrobead; Fig. 2 is the XRD figure of the molybdic oxide of the present embodiment preparation, and as can be seen from the figure, the diffraction peak position is consistent with molybdic oxide standard diffraction peak position, but diffraction peak intensity a little less than.
The ammonium dimolybdate material is pressed 1.4g/cm
2Be layed in (being to lay 1.4g ammonium dimolybdate material on every square centimeter of travelling belt) on the travelling belt, adopt travelling belt to drive the ammonium dimolybdate material and carry out calcination by calcination stove furnace chamber, calcination passes into the air flow line air opposite with the traffic direction of ammonium dimolybdate material with the flow velocity of 0.15m/s simultaneously in calcination stove furnace chamber, and air flow quantity is 12m3/h in the control calcination stove furnace chamber, and the rear naturally cooling of coming out of the stove 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 ℃, 430 ℃, 436 ℃, 468 ℃ and 460 ℃, and the length of calcination stove furnace chamber is 7000mm; Described ammonium dimolybdate material is 83min by the time of calcination stove furnace chamber.
The quality percentage composition of Mo is 66.55% in the molybdic oxide of the present embodiment preparation, and this molybdic oxide and phosphoric acid can rapid reactions, and the solution of generation is clarified, presented yellow-green colour, and without solid residue.
Fig. 3 is the SEM figure of the molybdic oxide of the present embodiment preparation, and as can be seen from the figure, the molybdic oxide particle becomes irregular bulk, uniform particles, and overall dimension is about 300 μ m, and large particle surface is adhering to fine particle; Fig. 4 is the XRD figure of the molybdic oxide of the present embodiment preparation, and as can be seen from the figure, the diffraction peak position is consistent with molybdic oxide standard diffraction peak position, but diffraction peak intensity is stronger.
The ammonium dimolybdate material is pressed 1.2g/cm
2Be layed in (being to lay 1.2g ammonium dimolybdate material on every square centimeter of material boat) on the material boat, adopt the material boat to drive the ammonium dimolybdate material and carry out calcination by calcination stove furnace chamber, calcination passes into the air flow line air opposite with the traffic direction of ammonium dimolybdate material with the flow velocity of 0.10m/s simultaneously in calcination stove furnace chamber, and air flow quantity is 8m in the control calcination stove furnace chamber
3/ h, the rear naturally cooling of coming out of the stove 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 ℃, 380 ℃, 430 ℃, 460 ℃ and 460 ℃, and the length of calcination stove furnace chamber is 7000mm; Described ammonium dimolybdate material is 120min by the time of calcination stove furnace chamber.
The quality percentage composition of Mo is 66.56% in the molybdic oxide of the present embodiment preparation, and this molybdic oxide and phosphoric acid can rapid reactions, and the solution of generation is clarified, presented glassy yellow, and without solid residue.
Fig. 5 is the SEM figure of the molybdic oxide of the present embodiment preparation, and as can be seen from the figure, the molybdic oxide particle is sharp-featured bulk, uniform particles, and overall dimension is about 650 μ m, and large particle surface is coarse, does not almost adhere to fine particle; Fig. 6 is the XRD figure of the molybdic oxide of the present embodiment preparation, and as can be seen from the figure, the diffraction peak position is consistent with molybdic oxide standard diffraction peak position, but diffraction peak intensity is stronger.
Embodiment 4
The ammonium dimolybdate material is pressed 1.4g/cm
2Be layed in (being to lay 1.4g ammonium dimolybdate material on every square centimeter of travelling belt) on the travelling belt, adopt travelling belt to drive the ammonium dimolybdate material and carry out calcination by calcination stove furnace chamber, calcination passes into the air flow line air opposite with the traffic direction of ammonium dimolybdate material with the flow velocity of 0.10m/s simultaneously in calcination stove furnace chamber, and air flow quantity is 8m3/h in the control calcination stove furnace chamber, and the rear naturally cooling of coming out of the stove 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 ℃, 380 ℃, 430 ℃, 460 ℃ and 460 ℃, and the length of calcination stove furnace chamber is 7000mm; Described ammonium dimolybdate material is 96min by the time of calcination stove furnace chamber.
The quality percentage composition of Mo is 66.55% in the molybdic oxide of the present embodiment preparation, and this molybdic oxide and phosphoric acid can rapid reactions, and the solution of generation is clarified, presented glassy yellow, and without solid residue.
Fig. 7 is the SEM figure of the molybdic oxide of the present embodiment preparation, and as can be seen from the figure, the molybdic oxide particle is sharp-featured bulk, uniform particles, overall dimension is about 650 μ m, 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 the molybdic oxide of the present embodiment preparation, and as can be seen from the figure, the diffraction peak position is consistent with molybdic oxide standard diffraction peak position, and diffraction peak intensity is than embodiment the last 3.
Embodiment 5
The ammonium dimolybdate material is pressed 1.4g/cm
2Be layed in (being to lay 1.4g ammonium dimolybdate material on every square centimeter of material boat) on the material boat, adopt the material boat to drive the ammonium dimolybdate material and carry out calcination by calcination stove furnace chamber, calcination passes into the air flow line air opposite with the traffic direction of ammonium dimolybdate material with the flow velocity of 0.19m/s simultaneously in calcination stove furnace chamber, and air flow quantity is 16m in the control calcination stove furnace chamber
3/ h, the rear naturally cooling of coming out of the stove 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 ℃, 430 ℃, 436 ℃, 468 ℃ and 460 ℃, and the length of calcination stove furnace chamber is 7000mm; Described ammonium dimolybdate material is 55min by the time of calcination stove furnace chamber.
The quality percentage composition of Mo is 66.62% in the molybdic oxide of the present embodiment preparation, and this molybdic oxide and phosphoric acid can rapid reactions, and the solution of generation is clarified, presented glassy yellow, and without solid residue.
Fig. 9 is the SEM figure of the molybdic oxide of the present embodiment preparation, and as can be seen from the figure, the molybdic oxide particle is sharp-featured bulk, uniform particles, and overall dimension is about 500 μ m, and large particle surface is coarse; Figure 10 is the XRD figure of the molybdic oxide of the present embodiment preparation, and as can be seen from the figure, the diffraction peak position is consistent with molybdic oxide standard diffraction peak position, and diffraction peak intensity is than embodiment the last 5.
Embodiment 6
The ammonium dimolybdate material is pressed 2.5g/cm
2Be layed in (being to lay 2.5g ammonium dimolybdate material on every square centimeter of travelling belt) on the travelling belt, adopt travelling belt to drive the ammonium dimolybdate material and carry out calcination by calcination stove furnace chamber, calcination passes into the air flow line air opposite with the traffic direction of ammonium dimolybdate material with the flow velocity of 0.50m/s simultaneously in calcination stove furnace chamber, and air flow quantity is 16m3/h in the control calcination stove furnace chamber, and the rear naturally cooling of coming out of the stove 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 ℃, 430 ℃, 436 ℃, 468 ℃ and 460 ℃, and the length of calcination stove furnace chamber is 7000mm; Described ammonium dimolybdate material is 83min by the time of calcination stove furnace chamber.
The quality percentage composition of Mo is 66.60% in the molybdic oxide of the present embodiment preparation, and this molybdic oxide and phosphoric acid can rapid reactions, and the solution of generation is clarified, presented glassy yellow, and without solid residue.
Figure 11 is the SEM figure of the molybdic oxide of the present embodiment preparation, and as can be seen from the figure, the molybdic oxide particle is sharp-featured bulk, uniform particles, and overall dimension is about 500 μ m, and large particle surface is coarse; Figure 12 is the XRD figure of the molybdic oxide of the present embodiment preparation, and as can be seen from the figure, the diffraction peak position is different from embodiment 1 to embodiment 5, and 2 θ angles are to occur an obvious diffraction peak near 13 °, and each diffraction peak intensity is the strongest among all embodiment simultaneously.
Element to the molybdic oxide of embodiment 1 to embodiment 6 preparation is analyzed, and 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 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, adopt the molybdic oxide constituent content of method calcination preparation of the present invention close, loose density is 1.43g/cm
3, Fisher particle size is 13.2 μ m, the basic indifference of constituent content.
The above; it only is preferred embodiment of the present invention; be not that the present invention is done any restriction, every any simple modification, change and equivalent structure of above embodiment being done according to the invention technical spirit changes, and all still belongs in the protection domain of technical solution of the present invention.
Claims (7)
1. a calcination ammonium dimolybdate prepares the method for molybdic oxide, it is characterized in that, the method is: the ammonium dimolybdate material is layed on material boat or the travelling belt, adopt material boat or travelling belt to drive the ammonium dimolybdate material and 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, the rear naturally cooling of coming out of the stove obtains molybdic oxide; The warm area of described calcination stove furnace chamber is distributed as 380 ℃～468 ℃; Described ammonium dimolybdate material is 55min～120min by the time of calcination stove furnace chamber; The air flow line of described air is opposite with the traffic direction of ammonium dimolybdate material.
2. a kind of calcination ammonium dimolybdate according to claim 1 prepares the method for molybdic oxide, it is characterized in that, the laying amount of described ammonium dimolybdate material is 1.2g/cm
2～2.5g/cm
2
3. a kind of calcination ammonium dimolybdate according to claim 1 prepares the method for molybdic oxide, it is characterized in that, air flow quantity is 8m in the described calcination stove furnace chamber
3/ h～16m
3/ h.
4. a kind of calcination ammonium dimolybdate according to claim 1 prepares the method for molybdic oxide, it is characterized in that, the warm area of described calcination stove furnace chamber is distributed as five warm areas.
5. a kind of calcination ammonium dimolybdate according to claim 4 prepares the method for molybdic oxide, it is characterized in that, the temperature of described five warm areas is followed successively by 380 ℃, 430 ℃, 436 ℃, 468 ℃ and 460 ℃.
6. a kind of calcination ammonium dimolybdate according to claim 4 prepares the method for molybdic oxide, it is characterized in that, the temperature of described five warm areas is followed successively by 380 ℃, 380 ℃, 430 ℃, 460 ℃ and 460 ℃.
7. 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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Cited By (2)
| 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 |
| 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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| 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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2012
- 2012-11-12 CN CN201210451912.1A patent/CN102897840B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Cited By (2)
| 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 |
| 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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