CN112850790A - Molybdenum trioxide for high-solubility catalyst and production process thereof - Google Patents
Molybdenum trioxide for high-solubility catalyst and production process thereof Download PDFInfo
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- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 title claims abstract description 200
- 239000003054 catalyst Substances 0.000 title claims abstract description 35
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- 238000001354 calcination Methods 0.000 claims abstract description 143
- XUFUCDNVOXXQQC-UHFFFAOYSA-L azane;hydroxy-(hydroxy(dioxo)molybdenio)oxy-dioxomolybdenum Chemical compound N.N.O[Mo](=O)(=O)O[Mo](O)(=O)=O XUFUCDNVOXXQQC-UHFFFAOYSA-L 0.000 claims abstract description 50
- 239000002245 particle Substances 0.000 claims abstract description 48
- 239000013078 crystal Substances 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 20
- 230000008569 process Effects 0.000 claims abstract description 20
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000002994 raw material Substances 0.000 abstract description 19
- 239000000463 material Substances 0.000 abstract description 10
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- 238000009826 distribution Methods 0.000 abstract description 7
- 238000006481 deamination reaction Methods 0.000 abstract description 6
- 230000009615 deamination Effects 0.000 abstract description 5
- 230000002829 reductive effect Effects 0.000 abstract description 5
- 230000018044 dehydration Effects 0.000 abstract description 4
- 238000006297 dehydration reaction Methods 0.000 abstract description 4
- 238000002425 crystallisation Methods 0.000 abstract description 2
- 230000008025 crystallization Effects 0.000 abstract description 2
- 238000012423 maintenance Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 21
- 230000000052 comparative effect Effects 0.000 description 19
- 239000012535 impurity Substances 0.000 description 17
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 16
- QXYJCZRRLLQGCR-UHFFFAOYSA-N dioxomolybdenum Chemical compound O=[Mo]=O QXYJCZRRLLQGCR-UHFFFAOYSA-N 0.000 description 12
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 6
- 239000006227 byproduct Substances 0.000 description 5
- 238000004090 dissolution Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 4
- 229940010552 ammonium molybdate Drugs 0.000 description 4
- 235000018660 ammonium molybdate Nutrition 0.000 description 4
- 239000011609 ammonium molybdate Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 235000019580 granularity Nutrition 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/02—Oxides; Hydroxides
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Catalysts (AREA)
Abstract
The invention provides a production process of molybdenum trioxide for a high-solubility catalyst, which comprises the following steps: s1, selecting single crystal ammonium dimolybdate with a specified particle size range, S2, placing the single crystal ammonium dimolybdate obtained in the step S1 into a rotary calcining furnace for calcining, wherein the rotary calcining furnace is divided into a low-temperature region and a high-temperature region, and finally taking out and cooling to obtain the single crystal ammonium dimolybdate, the particle size range of the single crystal ammonium dimolybdate is x micrometers-y micrometers, x is more than or equal to 80 and less than or equal to 160, y is more than or equal to 120 and less than or equal to 200, and y; according to the production process of the molybdenum trioxide for the high-solubility catalyst, the raw materials with narrow particle size distribution range are selected, so that the crystal growth process of the materials at a high temperature section is easy to control, and the obtained molybdenum trioxide has good crystal morphology and good solubility; and the deamination dehydration process and the molybdenum trioxide crystallization process are both put in a rotary calcining furnace for reaction, so that the process flow is simplified, the reaction equipment is simplified, the equipment maintenance cost is reduced, and the production cost of the product is saved.
Description
Technical Field
The invention relates to the technical field of metal materials, in particular to molybdenum trioxide for a high-solubility catalyst and a production process thereof.
Background
In the petroleum catalyst industry, the high-solubility molybdenum trioxide is a main raw material of various series of catalysts, and after being dissolved in water, the high-solubility molybdenum trioxide is adhered to the inner walls of pores of a porous medium to play a catalytic role.
The current molybdenum trioxide product mainly has three problems:
1. the product stability is poor mainly due to poor stability of the raw material ammonium molybdate and laggard production process;
2. the product has single type, only can be adapted to raw materials by customers, and basically can not produce personalized products according to the requirements of the customers;
3. the product has poor solubility, mainly reflects that the dissolution speed is slow, the components of the solution are complex after dissolution, and the insoluble substances are mainly caused: 1) the problems of agglomeration, wide particle size distribution and the like of the ammonium molybdate serving as a raw material exist, so that the calcined molybdenum trioxide is partially over-burnt and partially under-burnt; 2) the dissolution processes of all manufacturers are inconsistent, and corresponding calcination processes and corresponding ammonium molybdate physicochemical requirements are not developed.
Content of application
The invention aims to provide molybdenum trioxide for a high-solubility catalyst and a production process thereof, and the technical problem is effectively solved.
The embodiment of the invention is realized by the following technical scheme:
the invention provides a production process of molybdenum trioxide for a high-solubility catalyst, which comprises the following steps:
s1, selecting single crystal ammonium dimolybdate with specified particle size range;
s2, putting the single crystal ammonium dimolybdate obtained in the step S1 into a rotary calcining furnace for calcining, wherein the rotary calcining furnace is divided into a low-temperature area and a high-temperature area, and finally, taking out and cooling to obtain the single crystal ammonium dimolybdate;
wherein the particle size range of the single crystal ammonium dimolybdate is x micron-y micron;
wherein x is more than or equal to 80 and less than or equal to 160, y is more than or equal to 120 and less than or equal to 200, and y-x is less than or equal to 40.
The second aspect of the present invention provides molybdenum trioxide for a high-solubility catalyst produced by the above production process.
The technical scheme of the embodiment of the invention at least has the following advantages and beneficial effects:
according to the production process of the molybdenum trioxide for the high-solubility catalyst, the raw materials with narrow particle size distribution range are selected, and then the temperature and other parameters in the rotary furnace are adjusted according to the raw materials with different particle sizes, so that the heating process is easy to control, the crystal growth process of the materials at a high temperature section is easy to control, the obtained molybdenum trioxide is good in crystal morphology and good in solubility; in the second aspect, the production process provided by the invention has the advantages that the deamination dehydration process and the molybdenum trioxide crystallization process are both put in a rotary calcining furnace for reaction, so that the process flow is simplified, the reaction equipment is simplified, the equipment maintenance cost is reduced, and the production cost of the product is saved; in a third aspect, the production process provided by the invention can also produce various types of high-solubility molybdenum trioxide products according to specific requirements of customers, and the adaptability of the products is improved.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The present embodiment provides a process for producing molybdenum trioxide for highly soluble catalysts, which is used for preparing molybdenum trioxide for highly soluble catalysts, and comprises the following two steps (S1 and S2):
s1, selecting single crystal ammonium dimolybdate with specified particle size range;
wherein the particle size range of the single crystal ammonium dimolybdate is x micron-y micron;
wherein x is more than or equal to 80 and less than or equal to 160, y is more than or equal to 120 and less than or equal to 200, and y-x is less than or equal to 40.
So set up the particle size distribution that makes the ammonium dimolybdate as the raw materials comparatively concentrate, thereby can not produce the condition that one part ammonium dimolybdate overburnt another part ammonium dimolybdate is short of burning and causes the gained product solubility poor when calcining, in addition, reasonable particle size can avoid the raw materials on the one hand because the particle size is too little, cause mobility poor, and then the condition such as disconnected material takes place when the feed, on the other hand can avoid the raw materials because the particle size is too big, cause the outside of granule to overburnt and the condition that inside is short of burning when calcining.
Further, the particle size range of the single crystal ammonium dimolybdate is: one of 80 microns to 120 microns, 120 microns to 160 microns, and 160 microns to 200 microns.
And S2, putting the single crystal ammonium dimolybdate obtained in the step S1 into a rotary calcining furnace for calcining, wherein the rotary calcining furnace is divided into a low-temperature area and a high-temperature area, and finally taking out and cooling to obtain the single crystal ammonium dimolybdate.
The rotary calcining furnace is internally provided with 6 heating belts, each heating belt has the length of 700 mm and is divided into a belt, a second belt, a third belt, a fourth belt, a fifth belt and a sixth belt along the material conveying direction, wherein one zone and the two zones are low-temperature zones which are used for maintaining the dehydration deamination process of ammonium dimolybdate, the ammonium dimolybdate is decomposed in the low temperature region to generate water vapor and ammonia gas, and the ammonia gas can not be decomposed to generate reductive gas due to lower temperature, thereby effectively avoiding the molybdenum trioxide from self-reduction to generate by-products such as molybdenum dioxide and the like, the high temperature zone is from three zones to six zones, the high-temperature zone has the functions of controlling the particle growth size of the molybdenum trioxide (the growth degree of the molybdenum trioxide particles influences the dissolution performance thereof) by setting specific temperature, molybdenum trioxide products with different growth degrees and different solubility properties can be obtained by adjusting different temperature parameters.
The inclination of the furnace body of the rotary calcining furnace is 10-20 degrees, the reaction time of decomposing and roasting molybdenum trioxide by ammonium molybdate is adjusted by adjusting the rotating speed of the furnace tube, and the raw materials with various granularities are ensured to generate molybdenum trioxide completely, and the phase components are single.
By adjusting the feeding speed, the material layer thickness in the furnace is moderate, so as to ensure the uniform reaction of the molybdenum trioxide.
The furnace door is closed, the air pipe of the furnace end is provided with a fan for exhausting air in the furnace, the micro negative pressure in the furnace is adjusted through the frequency of the fan, and the air quantity of the exhausted air is maintained to be 500-1500 m when ammonium dimolybdate is calcined3And h, the generated water vapor and ammonia gas are timely pumped away, the phenomenon that the residual water vapor and ammonia gas in the furnace are decomposed into hydrogen gas to cause the self-reduction of the molybdenum trioxide to generate molybdenum dioxide is avoided, and meanwhile, the phenomenon that the materials in the furnace are pumped away to cause the reduction of the direct yield is avoided.
The temperature control, the furnace tube rotating speed, the feeding speed, the fan frequency and the like are monitored and adjusted by a PLC system, and the manual intervention is less.
Furthermore, the temperature of the low-temperature zone in the rotary calcining furnace is 400-460 ℃, the temperature of the high-temperature zone in the rotary calcining furnace is 440-530 ℃, the rotating speed of the rotary calcining furnace is 3-6 r/min, and the feeding speed of the rotary calcining furnace is 70-120 kg/h.
If the particle size range of the single crystal ammonium dimolybdate is 80-120 microns, the temperature of a low-temperature region in the rotary calcining furnace is 400-460 ℃, the temperature of a high-temperature region in the rotary calcining furnace is 440-520 ℃, the rotating speed of the rotary calcining furnace is 5-6 r/min, and the feeding speed of the rotary calcining furnace is 100-120 kg/h;
when the temperature of a low-temperature zone in the rotary calcining furnace is 400 ℃, the temperature of a high-temperature zone in the rotary calcining furnace is 440 ℃, the rotating speed of a converter of the rotary calcining furnace is 5r/min-6r/min, and the feeding speed of the rotary calcining furnace is 100kg/h-120kg/h, the dark gray molybdenum trioxide is prepared;
when the temperature of a low-temperature zone in the rotary calcining furnace is 440 ℃, the temperature of a high-temperature zone in the rotary calcining furnace is 470 ℃, the rotating speed of a converter of the rotary calcining furnace is 5r/min-6r/min, and the feeding speed of the rotary calcining furnace is 100kg/h-120kg/h, the light gray molybdenum trioxide is prepared;
when the temperature of a low-temperature zone in the rotary calcining furnace is 460 ℃, the temperature of a high-temperature zone in the rotary calcining furnace is 520 ℃, the rotating speed of a converter of the rotary calcining furnace is 5r/min-6r/min, and the feeding speed of the rotary calcining furnace is 100kg/h-120kg/h, the white molybdenum trioxide is prepared.
If the particle size range of the single crystal ammonium dimolybdate is 120-160 microns, the temperature of a low-temperature region in the rotary calcining furnace is 400-460 ℃, the temperature of a high-temperature region in the rotary calcining furnace is 445-525 ℃, the rotating speed of the rotary calcining furnace is 4-5 r/min, and the feeding speed of the rotary calcining furnace is 90-110 kg/h;
when the temperature of a low-temperature zone in the rotary calcining furnace is 400 ℃, the temperature of a high-temperature zone in the rotary calcining furnace is 445 ℃, the rotating speed of a converter of the rotary calcining furnace is 4r/min-5r/min, and the feeding speed of the rotary calcining furnace is 90kg/h-110kg/h, the dark gray molybdenum trioxide is prepared;
when the temperature of a low-temperature zone in the rotary calcining furnace is 440 ℃, the temperature of a high-temperature zone in the rotary calcining furnace is 475 ℃, the rotating speed of a converter of the rotary calcining furnace is 4r/min-5r/min, and the feeding speed of the rotary calcining furnace is 90kg/h-110kg/h, the light gray molybdenum trioxide is prepared;
when the temperature of the low-temperature zone in the rotary calcining furnace is 460 ℃, the temperature of the high-temperature zone in the rotary calcining furnace is 525 ℃, the rotating speed of the rotary calcining furnace is 4r/min-5r/min, and the feeding speed of the rotary calcining furnace is 90kg/h-110kg/h, the white molybdenum trioxide is prepared.
If the particle size range of the single crystal ammonium dimolybdate is 160-200 microns, the temperature of a low-temperature region in the rotary calcining furnace is 400-460 ℃, the temperature of a high-temperature region in the rotary calcining furnace is 460-530 ℃, the rotating speed of the rotary calcining furnace is 3-4 r/min, and the feeding speed of the rotary calcining furnace is 70-90 kg/h.
When the temperature of a low-temperature zone in the rotary calcining furnace is 400 ℃, the temperature of a high-temperature zone in the rotary calcining furnace is 460 ℃, the rotating speed of a converter of the rotary calcining furnace is 3r/min-4r/min, and the feeding speed of the rotary calcining furnace is 70kg/h-90kg/h, the dark gray molybdenum trioxide is prepared;
when the temperature of a low-temperature zone in the rotary calcining furnace is 440 ℃, the temperature of a high-temperature zone in the rotary calcining furnace is 495 ℃, the rotating speed of a converter of the rotary calcining furnace is 3r/min-4r/min, and the feeding speed of the rotary calcining furnace is 70kg/h-90kg/h, the light gray molybdenum trioxide is prepared;
when the temperature of the low-temperature zone in the rotary calcining furnace is 460 ℃, the temperature of the high-temperature zone in the rotary calcining furnace is 530 ℃, the rotating speed of the rotary calcining furnace is 3r/min-4r/min, and the feeding speed of the rotary calcining furnace is 70kg/h-90kg/h, the white molybdenum trioxide is prepared.
Example 1
Selecting ammonium dimolybdate with particle size ranging from 80 micrometers to 120 micrometers, feeding the ammonium dimolybdate into a rotary calcining furnace (with furnace body inclined at 10 degrees), closing a furnace door, arranging a fan on a furnace end air pipe to exhaust air in the furnace, adjusting micro negative pressure in the furnace through fan frequency, and maintaining the air volume of the exhaust air to be 1000m when calcining the ammonium dimolybdate3And/h, setting relevant parameters of a rotary calcining furnace through a PLC system, wherein the rotating speed of the rotary calcining furnace is 6r/min, the feeding speed of the rotary calcining furnace is 120kg/h, the temperature of a low-temperature zone in the rotary calcining furnace is 400 ℃, the temperature of a high-temperature zone is 440 ℃, and preparing the molybdenum trioxide A1 for the high-solubility catalyst.
Example 2
The remaining characteristics were the same as in example 1, except that the temperature in the low temperature zone was 440 ℃, the temperature in the high temperature zone was 470 ℃, the converter speed of the rotary calciner was 5r/min, and the feed rate of the rotary calciner was 110kg/h, to obtain molybdenum trioxide A2 for the highly soluble catalyst.
Example 3
The remaining characteristics were the same as in example 1, except that the temperature in the low temperature zone was 460 ℃, the temperature in the high temperature zone was 520 ℃, the converter speed of the rotary calciner was 5r/min, and the feed rate of the rotary calciner was 100kg/h, to obtain molybdenum trioxide A3 for the highly soluble catalyst.
Example 4
Selecting ammonium dimolybdate with particle size of 120-160 microns, feeding into a rotary calciner (inclined at 15 degree) with furnace body, closing furnace door, arranging fan at furnace end air pipe to exhaust air, regulating micro negative pressure in the calciner via fan frequency, and maintaining exhaust air volume at 1000m when calcining ammonium dimolybdate3Setting relevant parameters of a rotary calcining furnace through a PLC system, wherein the rotating speed of the rotary calcining furnace is 5r/min, the feeding speed of the rotary calcining furnace is 110kg/h,the temperature of the low-temperature zone in the rotary calcining furnace is 400 ℃, and the temperature of the high-temperature zone is 445 ℃, so that the molybdenum trioxide A4 for the high-solubility catalyst is prepared.
Example 5
The remaining characteristics were the same as in example 4, except that the temperature in the low temperature zone was 440 ℃, the temperature in the high temperature zone was 475 ℃, the converter speed of the rotary calciner was 4r/min, and the feed rate of the rotary calciner was 100kg/h, to obtain molybdenum trioxide A5 for the highly soluble catalyst.
Example 6
The remaining characteristics were the same as in example 4, except that the temperature in the low temperature zone was 460 ℃, the temperature in the high temperature zone was 525 ℃, the converter speed of the rotary calciner was 4r/min, and the feed rate of the rotary calciner was 90kg/h, to obtain molybdenum trioxide A6 for the highly soluble catalyst.
Example 7
Selecting ammonium dimolybdate with particle size range of 160-200 microns, feeding into a rotary calcining furnace (furnace body inclination angle is 10 °), closing furnace door, configuring fan on furnace end air pipe to exhaust air in the furnace, regulating micro negative pressure in the furnace through fan frequency, and maintaining exhaust air volume at 1000m when calcining ammonium dimolybdate3And/h, setting relevant parameters of a rotary calcining furnace through a PLC system, wherein the rotating speed of the rotary calcining furnace is 3r/min, the feeding speed of the rotary calcining furnace is 70kg/h, the temperature of a low-temperature zone in the rotary calcining furnace is 400 ℃, the temperature of a high-temperature zone is 460 ℃, and preparing the molybdenum trioxide A7 for the high-solubility catalyst.
Example 8
The remaining characteristics were the same as in example 7, except that the temperature in the low temperature zone was 440 ℃, the temperature in the high temperature zone was 495 ℃, the converter speed of the rotary calciner was 4r/min, and the feed rate of the rotary calciner was 80kg/h, to obtain molybdenum trioxide A8 for the highly soluble catalyst.
Example 9
The remaining characteristics were the same as in example 7, except that the temperature in the low temperature zone was 460 ℃, the temperature in the high temperature zone was 530 ℃, the converter speed of the rotary calciner was 4r/min, and the feed rate of the rotary calciner was 90kg/h, to obtain molybdenum trioxide A9 for the highly soluble catalyst.
Comparative example 1
The remaining characteristics were the same as in example 1, except that ammonium dimolybdate having a particle size of less than 10 microns was used, and molybdenum trioxide D1 was finally produced.
Comparative example 2
The remaining characteristics were the same as in example 1, except that ammonium dimolybdate having a particle size of greater than 300 microns was used to produce molybdenum trioxide D2.
Comparative example 3
The remaining characteristics were the same as in example 1, except that ammonium dimolybdate having a particle size ranging from 30 microns to 120 microns (i.e., a broad particle size distribution) was used to produce molybdenum trioxide D3.
Comparative example 4
The remaining characteristics were the same as in example 1, except that the temperature of the low-temperature zone in the rotary calciner was 200 ℃ to finally obtain molybdenum trioxide D4.
Comparative example 5
The remaining characteristics were the same as in example 1, except that the temperature of the low-temperature region was 440 ℃ as that of the high-temperature region, i.e., the low-temperature region and the high-temperature region were not distinguished, and finally molybdenum trioxide D5 was produced.
Comparative example 6
The remaining characteristics were the same as in example 1, except that the temperature of the low-temperature zone was 400 ℃ as the temperature of the high-temperature zone, i.e., the low-temperature zone and the high-temperature zone were not distinguished, and the calcination temperature was low, to finally obtain molybdenum trioxide D6.
Comparative example 7
The remaining characteristics were the same as in example 1, except that the temperature of the high-temperature zone was 550 ℃, and molybdenum trioxide D7 was finally obtained.
Comparative example 8
The rest characteristics are the same as those of the embodiment 1, except that the revolving speed of the revolving calciner is 8r/min, the feeding speed of the revolving calciner is 140kg/h, and finally, the molybdenum trioxide D8 is prepared.
Comparative example 9
The other characteristics are the same as those of the embodiment 1, except that the revolving speed of the revolving calciner is 4r/min, the feeding speed of the revolving calciner is 60kg/h, and finally, the molybdenum trioxide D9 is prepared.
Examples of the experiments
The solubility properties of the highly soluble catalysts obtained in examples 1 to 9 described above were recorded in the form of a characterization of the color of the solid powder and the solubility properties of the molybdenum trioxide A1-A9 and the molybdenum trioxide D1-D9 obtained in comparative examples 1 to 9.
The dissolution performance was tested as follows:
10 g of the finally obtained product is put into 100 ml of phosphoric acid solution, stirred and filtered, and if a solid substance is attached to the filter paper, the solid substance is dried and weighed to obtain x g, and the solubility of the product is (10-x)/10 x 100%.
The experimental data are shown in table 1 below.
TABLE 1 molybdenum trioxide solubility Properties and color
As can be seen from Table 1, the molybdenum trioxide A1-A9 prepared in examples 1-9 has good solubility, indicating that ammonium dimolybdate is completely converted into molybdenum trioxide without impurities, because the ammonium dimolybdate used as a calcination raw material has a narrow particle size distribution and small particle size difference, and does not cause over-burning of one part of the material during calcination, and has a moderate particle size, so as to ensure the fluidity of the material during calcination and further ensure no material breakage, the prepared molybdenum trioxide product can be effectively loaded into the internal space of the porous material to play a catalytic role after being dissolved in phosphoric acid, and the reaction conditions (such as the temperature in the low temperature region and the temperature in the high temperature region) can be finely adjusted according to the requirements of customers to obtain products with different colors (such as deep ash, light ash and white), when a1 to a9 were dissolved in each of the phosphoric acid solutions, the resulting solutions were colored, but were clear and free from turbidity as a whole.
The molybdenum trioxide D1 prepared in the comparative example 1 has small fluidity due to the particle size of the selected ammonium dimolybdate being less than 10 microns, and is easy to bridge during feeding, so that the conditions of material breakage and the like can cause over-burning of part of raw materials and generation of yellow impurities, and because the particle size of the raw materials is too small, the raw materials are easy to adhere and decompose during reaction in a furnace to generate steam, so that the content of Fe in a finally fired product exceeds the standard, and after the raw materials are put into a phosphoric acid solution, effective components (molybdenum trioxide) are dissolved, and the yellow impurities are suspended in the solution, so that the solution becomes turbid and is difficult to transmit light.
The molybdenum trioxide D2 prepared in comparative example 2 has excessive particle size, when calcinating, the outer surface part of the ammonium dimolybdate is easy to be over-burned and the inner part is under-burned, i.e. the calcination is not uniform, the color of the final product is impure, wherein yellow is impurity generated by over-burning, gray is molybdenum trioxide, and black is impurity generated by under-burning, after the product is put into phosphoric acid solution, the gray molybdenum trioxide is completely dissolved, part of black impurity floats on the liquid surface, the other part of black impurity is accumulated and deposited at the bottom of the solution, and the yellow impurity is suspended in the solution, so that the solution becomes turbid and is not easy to transmit light.
The molybdenum trioxide D3 prepared in comparative example 3 has a wide particle size distribution of ammonium dimolybdate, i.e., the particles of the raw material have uneven sizes, particles with smaller particle sizes are over-burned during calcination to generate yellow impurities, particles with larger particle sizes are under-burned to generate black impurities, and after the product is put into a phosphoric acid solution, the gray molybdenum trioxide is completely dissolved, a part of the yellow or black impurities float on the liquid surface, the other part of the yellow or black impurities are accumulated and deposited at the bottom of the solution, and the yellow impurities are suspended in the solution, so that the solution becomes turbid and is not easy to transmit light.
According to the molybdenum trioxide D4 prepared in the comparative example 4, because the temperature of the low-temperature region is too low, only water vapor is removed, and deamination reaction or partial deamination does not occur, so that ammonium dimolybdate is deaminated in the high-temperature region, and ammonia gas generates reducing gas in a high-temperature environment, so that molybdenum trioxide is self-reduced to generate by-products such as molybdenum dioxide, and the like, and the finally obtained product powder presents alternate gray and black mixed colors, wherein gray is molybdenum trioxide and black is by-products such as molybdenum dioxide, and after the product is put into phosphoric acid, molybdenum trioxide is dissolved, and the by-products such as molybdenum dioxide are deposited at the bottom of the solution.
In the molybdenum trioxide D5 prepared in the comparative example 5, since a low temperature region is not set, the dehydration deamination process of ammonium dimolybdate is directly performed in a high temperature environment, and the generated ammonia gas is decomposed in the high temperature environment to generate reducing gas, so that the molybdenum trioxide is self-reduced to generate byproducts such as molybdenum dioxide.
The molybdenum trioxide D6 produced in comparative example 6 was partially under-burned due to a low temperature, and the resulting product exhibited a dark gray color, and after it was added to phosphoric acid, the gray molybdenum trioxide dissolved and black impurities suspended in the solution, making the solution cloudy.
The molybdenum trioxide D7 obtained in comparative example 7 was over-burned due to a high temperature, and a part of yellow impurities were generated.
The molybdenum trioxide D8 produced in comparative example 8 was fed too quickly, resulting in a partial under-burning of the raw material and a partial black impurity.
The molybdenum trioxide D9 produced in comparative example 9 was excessively slow in feeding, causing excessive burning of a part of the raw material, resulting in generation of a part of yellow impurities.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A production process of molybdenum trioxide for a high-solubility catalyst is characterized by comprising the following steps:
s1, selecting single crystal ammonium dimolybdate with specified particle size range;
s2, putting the single crystal ammonium dimolybdate obtained in the step S1 into a rotary calcining furnace for calcining, wherein the rotary calcining furnace is divided into a low-temperature area and a high-temperature area, and finally, taking out and cooling to obtain the single crystal ammonium dimolybdate;
wherein the particle size range of the single crystal ammonium dimolybdate is x micron-y micron;
wherein x is more than or equal to 80 and less than or equal to 160, y is more than or equal to 120 and less than or equal to 200, and y-x is less than or equal to 40.
2. The process for producing molybdenum trioxide for highly soluble catalysts according to claim 1, wherein the particle size of the single-crystal ammonium dimolybdate is in the range of: one of 80 microns to 120 microns, 120 microns to 160 microns, and 160 microns to 200 microns.
3. The process for producing molybdenum trioxide for highly soluble catalysts as claimed in claim 2, wherein the temperature of the low temperature zone in the rotary calciner is 400-460 ℃, the temperature of the high temperature zone in the rotary calciner is 440-530 ℃, the converter rotation speed of the rotary calciner is 3-6 r/min, and the feeding speed of the rotary calciner is 70-120 kg/h.
4. The process for producing molybdenum trioxide for a highly soluble catalyst according to claim 3, wherein:
if the particle size range of the single crystal ammonium dimolybdate is 80-120 microns, the temperature of a low-temperature region in the rotary calcining furnace is 400-460 ℃, the temperature of a high-temperature region in the rotary calcining furnace is 440-520 ℃, the rotating speed of the rotary calcining furnace is 5-6 r/min, and the feeding speed of the rotary calcining furnace is 100-120 kg/h;
if the particle size range of the single crystal ammonium dimolybdate is 120-160 microns, the temperature of a low-temperature region in the rotary calcining furnace is 400-460 ℃, the temperature of a high-temperature region in the rotary calcining furnace is 445-525 ℃, the rotating speed of the rotary calcining furnace is 4-5 r/min, and the feeding speed of the rotary calcining furnace is 90-110 kg/h;
if the particle size range of the single crystal ammonium dimolybdate is 160-200 microns, the temperature of a low-temperature region in the rotary calcining furnace is 400-460 ℃, the temperature of a high-temperature region in the rotary calcining furnace is 460-530 ℃, the rotating speed of the rotary calcining furnace is 3-4 r/min, and the feeding speed of the rotary calcining furnace is 70-90 kg/h.
5. The process for producing molybdenum trioxide for highly soluble catalysts according to claim 4, wherein if the particle size of the single-crystal ammonium dimolybdate is in the range of 80 to 120 μm:
when the temperature of a low-temperature zone in the rotary calcining furnace is 400 ℃, the temperature of a high-temperature zone in the rotary calcining furnace is 440 ℃, the rotating speed of a converter of the rotary calcining furnace is 5r/min-6r/min, and the feeding speed of the rotary calcining furnace is 100kg/h-120kg/h, the dark gray molybdenum trioxide is prepared;
when the temperature of a low-temperature zone in the rotary calcining furnace is 440 ℃, the temperature of a high-temperature zone in the rotary calcining furnace is 470 ℃, the rotating speed of a converter of the rotary calcining furnace is 5r/min-6r/min, and the feeding speed of the rotary calcining furnace is 100kg/h-120kg/h, the light gray molybdenum trioxide is prepared;
when the temperature of the low-temperature zone in the rotary calcining furnace is 460 ℃, the temperature of the high-temperature zone in the rotary calcining furnace is 520 ℃, the rotating speed of the rotary calcining furnace is 5r/min-6r/min, and the feeding speed of the rotary calcining furnace is 100kg/h-120kg/h, the white molybdenum trioxide is prepared.
6. The process for producing molybdenum trioxide for highly soluble catalysts according to claim 4, wherein if the particle size of the single-crystal ammonium dimolybdate is in the range of 120 to 160 μm:
when the temperature of the low-temperature zone in the rotary calcining furnace is 400 ℃, the temperature of the high-temperature zone in the rotary calcining furnace is 445 ℃, the rotating speed of a converter of the rotary calcining furnace is 4r/min-5r/min, and the feeding speed of the rotary calcining furnace is 90kg/h-110kg/h, the dark gray molybdenum trioxide is prepared;
when the temperature of the low-temperature zone in the rotary calcining furnace is 440 ℃, the temperature of the high-temperature zone in the rotary calcining furnace is 475 ℃, the rotating speed of a converter of the rotary calcining furnace is 4r/min-5r/min, and the feeding speed of the rotary calcining furnace is 90kg/h-110kg/h, the light gray molybdenum trioxide is prepared;
when the temperature of the low-temperature zone in the rotary calcining furnace is 460 ℃, the temperature of the high-temperature zone in the rotary calcining furnace is 525 ℃, the rotating speed of the rotary calcining furnace is 4r/min-5r/min, and the feeding speed of the rotary calcining furnace is 90kg/h-110kg/h, the white molybdenum trioxide is prepared.
7. The process for producing molybdenum trioxide for highly soluble catalysts according to claim 4, wherein if the particle size of the single-crystal ammonium dimolybdate is in the range of 160 to 200 μm:
when the temperature of a low-temperature zone in the rotary calcining furnace is 400 ℃, the temperature of a high-temperature zone in the rotary calcining furnace is 460 ℃, the rotating speed of a converter of the rotary calcining furnace is 3r/min-4r/min, and the feeding speed of the rotary calcining furnace is 70kg/h-90kg/h, the dark gray molybdenum trioxide is prepared;
when the temperature of a low-temperature zone in the rotary calcining furnace is 440 ℃, the temperature of a high-temperature zone in the rotary calcining furnace is 495 ℃, the rotating speed of a converter of the rotary calcining furnace is 3r/min-4r/min, and the feeding speed of the rotary calcining furnace is 70kg/h-90kg/h, so as to prepare light gray molybdenum trioxide;
when the temperature of the low-temperature zone in the rotary calcining furnace is 460 ℃, the temperature of the high-temperature zone in the rotary calcining furnace is 530 ℃, the rotating speed of the rotary calcining furnace is 3r/min-4r/min, and the feeding speed of the rotary calcining furnace is 70kg/h-90kg/h, the white molybdenum trioxide is prepared.
8. The process for producing molybdenum trioxide for a high-solubility catalyst in accordance with claim 2, wherein in step S2, the low temperature zone includes two heating zones and the high temperature zone includes four heating zones.
9. Molybdenum trioxide for highly soluble catalysts, characterized by being produced by the production process of molybdenum trioxide for highly soluble catalysts according to any one of claims 1 to 8.
10. The molybdenum trioxide for high-solubility catalyst according to claim 9, wherein the color of the molybdenum trioxide for high-solubility catalyst comprises: dark grey, light grey or white.
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