CN109775760B - Ultra-low potassium ammonium molybdate solution, ammonium molybdate solution derivative product and preparation method thereof - Google Patents
Ultra-low potassium ammonium molybdate solution, ammonium molybdate solution derivative product and preparation method thereof Download PDFInfo
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Abstract
The invention provides an ultra-low potassium ammonium molybdate solution, an ammonium molybdate solution derivative product and a preparation method thereof, belonging to the technical field of metallurgy. The potassium content in the ammonium molybdate solution provided by the invention can be controlled within 10ppm, and the derivative product of the ammonium molybdate solution is prepared from the ultra-low potassium ammonium molybdate solution and comprises ammonium dimolybdate, ammonium tetramolybdate, ammonium heptamolybdate and high-purity molybdenum trioxide. The preparation method of the ammonium molybdate solution derivative product mainly comprises the following steps: adsorbing the sodium molybdate solution by an ion exchange column; introducing the ammonia water solution into an ion exchange column with saturated adsorption for analysis to obtain an ultralow potassium ammonium molybdate solution; taking the production of ammonium dimolybdate as an example, evaporating and crystallizing the obtained ultra-low potassium ammonium molybdate solution to obtain ammonium dimolybdate, and then roasting to obtain molybdenum trioxide; and absorbing ammonia gas generated in the roasting process by pure water to obtain an ammonia water solution, and feeding the ammonia water solution into an ion exchange column for analysis. The preparation method is green and environment-friendly, and theoretical liquid ammonia consumption is zero.
Description
Technical Field
The invention belongs to the technical field of metallurgy, and particularly relates to an ultra-low potassium ammonium molybdate solution and a derivative product prepared by using the ultra-low potassium ammonium molybdate solution as a raw material.
Background
Ammonium molybdate is an important link of a molybdenum processing industrial chain, and is mainly used for preparing high-purity molybdenum trioxide and metal molybdenum powder so as to prepare molybdenum materials such as molybdenum alloy, molybdenum wires and the like; it is also an important chemical raw material, and is widely applied to industries such as metallurgy, chemical industry, catalysts and the like.
The traditional ammonium molybdate processing process generally comprises six procedures of acid salt pretreatment, ammonia leaching, acid precipitation, ammonia dissolution, evaporation and the like, and in the process, impurity elements in molybdenum calcine can be transferred into a solution and are not easy to remove, so that the performance of an ammonium molybdate product is influenced, wherein the influence of a potassium element on the performance of the ammonium molybdate product is particularly serious. The melting point of the potassium is 63 ℃, the boiling point of the potassium is 774 ℃, and when the ammonium molybdate product is used as a photoelectric source material in a high-temperature sintering process of a subsequent ammonium molybdate product (above 1900 ℃), the potassium can volatilize and adhere to a heating element or a luminous source device, and the insulating property of the heating element or the luminous source device is influenced after moisture absorption, or a strong alkali solution is formed to corrode the heating element or the luminous source device, so that pollution is caused. When ammonium molybdate products are added to the alloy, the potassium element also affects the mechanical and mechanical properties of the alloy, and therefore, how to obtain ammonium molybdate solution with low potassium content is very important in the industry chain of molybdenum processing.
In order to reduce the content of potassium in the ammonium molybdate solution, the prior art (CN108118148A) discloses a method for controlling the content of potassium in the ammonium molybdate solution, which comprises mixing high-potassium molybdenum calcine and low-potassium molybdenum calcine in proportion, washing with water, and leaching with ammonia to obtain the ammonium molybdate solution, wherein the content of potassium in the ammonium molybdate solution is 30mg/L-40mg/L, and the content of potassium in the generated ammonium dimolybdate is not less than 30. Another prior art (CN107986332A) discloses a potassium reduction method for an ammonium molybdate solution, which comprises washing molybdenum calcine with water, and filtering to obtain a filter cake; then putting the filter cake into ammonia water with the pH value of 8.0-9.0, carrying out ammonia leaching treatment, and filtering to obtain filtrate; and finally, aging the filtrate, and filtering to obtain an ammonium molybdate solution, wherein the potassium content in the ammonium molybdate solution is 22-27mg/L, and the potassium content in the generated ammonium dimolybdate is more than or equal to 30. Although the potassium content of the ammonium molybdate disclosed in the prior art can be reduced to about 30mg/L, in some high-end product applications, it is still desirable to control the potassium content to a lower level, i.e., to obtain an ultra-low potassium ammonium molybdate solution and to use the ultra-low potassium ammonium molybdate solution to produce ultra-low potassium ammonium molybdate.
In addition, a large amount of ammonia nitrogen wastewater can be generated in the existing production process of ammonium molybdate and molybdenum trioxide, the environmental pollution is serious, along with the increasing attention of the country on environmental protection, the development of a preparation process with zero wastewater and waste gas emission and zero theoretical consumption of liquid ammonia is very important.
Disclosure of Invention
In view of the above background problems, the present invention is directed to provide an ultra-low potassium ammonium molybdate solution, wherein the potassium content in the ammonium molybdate solution can be controlled within 10ppm, and the derived product can be obtained by processing the obtained ultra-low potassium ammonium molybdate solution. The invention also aims to provide the preparation method of the ammonium molybdate solution derivative product, which is green and environment-friendly and has zero theoretical liquid ammonia consumption.
To achieve the above object, the present invention provides:
the content of potassium in the ultra-low potassium ammonium molybdate solution is less than or equal to 10 ppm.
The invention also provides an ammonium molybdate solution derivative product which is prepared from the ultra-low potassium ammonium molybdate solution, and the potassium content in the ammonium molybdate solution derivative product is less than or equal to 10 ppm.
Wherein the ammonium molybdate solution derived products comprise ammonium dimolybdate, ammonium tetramolybdate, ammonium heptamolybdate and high-purity molybdenum trioxide.
In order to achieve the above object, the present invention further provides a method for preparing the ammonium molybdate derivative product, comprising the following steps:
s1, treating the molybdenum calcine with alkali liquor to obtain a sodium molybdate solution;
s2, adsorbing the sodium molybdate solution obtained in the step S1 by an ion exchange column;
s3, introducing the ammonia water solution into the ion exchange column with saturated adsorption in the step S2 for analysis to obtain an ultra-low potassium ammonium molybdate solution;
s4, evaporating and crystallizing the ultra-low potassium ammonium molybdate solution obtained in the S3 to obtain ammonium dimolybdate, and roasting to obtain high-purity molybdenum trioxide;
s5, introducing ammonia gas generated in the roasting process in the step S4 into an ammonia gas absorption tower, introducing pure water to absorb the ammonia gas to obtain an ammonia water solution, and allowing the obtained ammonia water solution to enter the ion exchange column in the step S3 for analysis so as to realize recycling.
Preferably, in the step S1, the molybdenum calcine is low-grade molybdenum calcine; the alkali liquor is sodium hydroxide, sodium carbonate or a combination of the sodium hydroxide and the sodium carbonate, and the pH value of the alkali liquor is more than 9.
Preferably, in the step S2, the sodium molybdate solution obtained in the step S1 is adsorbed by passing through a plurality of ion exchange columns connected in series in sequence.
More preferably, the ion exchange resin in the ion exchange column is a weakly basic anion exchange resin.
Preferably, in the step S5, the ammonia gas generated in the torrefaction process in the step S4 is introduced into a primary ammonia gas absorption tower and a secondary ammonia gas absorption tower which are sequentially communicated, the ammonia gas in the secondary ammonia gas absorption tower is absorbed by pure water to obtain dilute ammonia water, the obtained dilute ammonia water is returned to the primary ammonia gas absorption tower to be reabsorbed to obtain concentrated ammonia water, and finally the obtained concentrated ammonia water is returned to the ion exchange column to be analyzed.
More preferably, the concentration of the concentrated ammonia water is 3-5%, and the pH is 9-11.
Preferably, in the step of S2, the adsorption temperature is 30-50 ℃.
Compared with the prior art, the invention has the following effects:
1. the potassium content in the ultra-low potassium ammonium molybdate solution provided by the invention can be controlled below 10ppm, and the potassium content of a derivative product obtained by processing the ultra-low potassium ammonium molybdate solution can be controlled below 10ppm, so that the ultra-low potassium ammonium molybdate solution can be applied to a higher-end field, and the application range of the product is expanded; 2. the preparation method provided by the invention reduces the pretreatment process of the traditional ammonium molybdate process, ammonia gas is always carried out in a closed space in the whole production process, no ammonia gas escapes from the site, an ammonia water solution generated by an ammonia gas absorption tower returns to an ion exchange column to analyze molybdate ions, and no wastewater is discharged; 3. the ammonia gas generated in the roasting process is absorbed by a two-stage or multi-stage ammonia gas absorption tower, and the discharge port completely reaches the standard; 4. the invention can be produced and prepared by low-grade raw materials, thereby reducing the cost.
Drawings
Fig. 1 is a flow chart of a preparation process of an ultra-low potassium ammonium molybdate solution and a derivative product of the ammonium molybdate solution in the embodiment of the invention.
Detailed Description
The invention relates to the technical field of metallurgy, and mainly aims to provide an ultra-low potassium ammonium molybdate solution, wherein the potassium content in the ammonium molybdate solution can be controlled within 10ppm, ammonium molybdate solution derivative products are obtained by processing the ultra-low potassium ammonium molybdate solution, the ammonium molybdate solution derivative products comprise ammonium dimolybdate, ammonium tetramolybdate, ammonium heptamolybdate, high-purity molybdenum trioxide and the like, and the potassium content in the ammonium molybdate solution derivative products can be controlled within 10 ppm. When the ammonium molybdate solution derivative product is prepared (taking preparation of ammonium dimolybdate and molybdenum trioxide as examples), the method mainly comprises the following steps: s1, treating the molybdenum calcine with alkali liquor to obtain a sodium molybdate solution; s2, adsorbing the sodium molybdate solution obtained in the step S1 by an ion exchange column; s3, introducing the ammonia water solution into the ion exchange column with saturated adsorption in the step S2 for analysis to obtain an ultra-low potassium ammonium molybdate solution; s4, carrying out evaporative crystallization on the ultra-low potassium ammonium molybdate solution obtained in the step S3 to obtain ultra-low potassium ammonium dimolybdate, and then roasting to obtain high-purity molybdenum trioxide; s5, introducing ammonia gas generated in the roasting process in the step S4 into an ammonia gas absorption tower, introducing pure water to absorb the ammonia gas to obtain an ammonia water solution, and allowing the obtained ammonia water solution to enter the ion exchange column in the step S3 for analysis so as to realize recycling. The preparation method can be used for preparing ultralow-potassium ammonium dimolybdate and high-purity molybdenum trioxide, is environment-friendly, and has the advantages of closed production process and no waste water and waste gas emission.
The present invention will be described in detail with reference to the following specific examples, which are intended to illustrate the preparation of the derivative products in the following examples using ammonium dimolybdate and high purity molybdenum trioxide only, and for the preparation of ammonium tetramolybdate and ammonium heptamolybdate, the ammonium molybdate solution obtained is treated according to the conventional techniques.
Example 1
Calcining molybdenum in a reaction kettle: water 1 ton: 2m3Adding the molybdenum calcine and water according to the mixture ratio, then adding sodium carbonate to adjust the pH value to 9, and heating and reacting for one hour by utilizing steam to obtain a sodium molybdate solution. Discharging materials after the reaction is finished, performing filter pressing by using a filter, and storing clear liquid after the filter pressing in a buffer container. And (3) sequentially introducing the sodium molybdate solution in the buffer tank into ion exchange columns 1, 2 and 3 connected in series by using a centrifugal pump for adsorption, wherein D314 exchange resin is selected in the ion exchange columns, and the adsorption temperature is 30 ℃. In specific use, the adsorbed waste liquid can be used for preparing industrial salt through an evaporation system. After the ion exchange columns 1, 2 and 3 are saturated in adsorption, the ammonium molybdate solution with ultralow potassium content can be obtained by resolving with an ammonia water solution with the concentration of 4%.
And then concentrating the ammonium molybdate solution, then pumping the concentrated ammonium molybdate solution into a crystallizer, carrying out evaporation crystallization on the material at the evaporation temperature of less than 101 ℃ to obtain ammonium dimolybdate, centrifugally drying the ammonium dimolybdate, and then feeding the ammonium dimolybdate into a roasting furnace at the roasting temperature of 300-600 ℃, thus obtaining a reagent-grade high-purity molybdenum trioxide product by roasting. The ammonia can be produced in the roasting process, in order to realize no waste gas emission, the produced ammonia sequentially passes through the primary ammonia absorption tower and the secondary ammonia absorption tower, the unabsorbed ammonia of the primary ammonia absorption tower enters the secondary ammonia absorption tower, and is absorbed by pure water to obtain secondary ammonia water, and at the moment, the tail gas of the secondary absorption tower only has a very small amount of ammonia and is absorbed by a sulfuric acid solution, so that zero emission of the ammonia is realized. And the secondary ammonia water obtained in the secondary ammonia absorption tower returns to the primary ammonia absorption tower to be reabsorbed to obtain primary ammonia water, the obtained primary ammonia water is used for the analysis process, and in addition, the ammonia water generated in the evaporation process of the ammonium molybdate solution can also be used for the analysis process, so that the cyclic recycling is realized. The specific flow process is shown in the process diagram in figure 1.
In the above preparation process, the following reaction principle exists:
(1) dissolving sodium carbonate in water to form an alkaline solution, putting molybdenum calcine into the solution to form a sodium molybdate solution, wherein the chemical reaction equation is as follows:
MoO3+H2O→H2MoO4
Na2CO3+H2MoO4→Na2MoO4+H2O+CO2
(2) ammonium hydroxide is utilized to resolve molybdate ions in the ion exchange resin to form ammonium molybdate solution, and the chemical reaction equation is as follows:
Na2MoO4+2NH4OH→(NH4)2MoO4+2NaOH
NaOH+HCl→NaCl+H2O
(3) ammonium dimolybdate crystals are obtained from the ammonium molybdate solution by using the evaporative crystallization principle.
2(NH4)2MoO4→(NH4)2MO2O7+2NH3+H2O
(4) Ammonium dimolybdate is utilized to calcine and decompose to generate high-purity molybdenum trioxide, and the chemical reaction equation is as follows:
(NH4)2Mo2O7→2MoO3+2NH3+H2O
example 2
Calcining molybdenum in a reaction kettle: water 1 ton: 3m3Adding the molybdenum calcine and water according to the mixture ratio, then adding sodium carbonate to adjust the pH value to 10, and heating and reacting for one hour by utilizing steam to obtain a sodium molybdate solution. Discharging materials after the reaction is finished, performing filter pressing by using a filter, and storing clear liquid after the filter pressing in a buffer container. And (3) sequentially introducing the sodium molybdate solution in the buffer tank into ion exchange columns 1, 2 and 3 connected in series by using a centrifugal pump for adsorption, wherein D314 exchange resin is selected in the ion exchange columns, the adsorption temperature is 40 ℃, and after the ion exchange columns 1, 2 and 3 are saturated in adsorption, the ammonium molybdate solution with ultralow potassium content can be obtained by resolving with an ammonia water solution with the concentration of 3%. The subsequent torrefaction and ammonia gas recovery process was the same as in example 1.
Example 3
Calcining molybdenum in a reaction kettle: water 1 ton: 4m3Adding the molybdenum calcine and water according to the mixture ratio, then adding sodium carbonate to adjust the pH value to 11, and heating and reacting for one hour by utilizing steam to obtain a sodium molybdate solution. Discharging materials after the reaction is finished, performing filter pressing by using a filter, and storing clear liquid after the filter pressing in a buffer container. And (3) sequentially introducing the sodium molybdate solution in the buffer tank into ion exchange columns 1, 2 and 3 connected in series by using a centrifugal pump for adsorption, wherein D314 exchange resin is selected in the ion exchange columns, the adsorption temperature is 50 ℃, and after the ion exchange columns 1, 2 and 3 are saturated in adsorption, the ammonium molybdate solution with ultralow potassium content can be obtained by resolving with an ammonia water solution with the concentration of 5%. The subsequent torrefaction and ammonia gas recovery process was the same as in example 1.
The ammonium molybdate solution, ammonium dimolybdate, high-purity molybdenum trioxide and the existing products prepared in examples 1 to 3 were subjected to potassium content and other impurity content measurement mainly by an atomic absorption spectrometer and an inductively coupled plasma emission spectrometer, and the test method is prior art and will not be described herein again. Wherein, the existing products are respectively produced by the Fukucheng molybdenum industry group and the Xinhualong molybdenum industry Co. The test results are shown in tables 1-3.
Table 1 various impurities and their contents in ammonium molybdate solutions in examples 1-3
TABLE 2 ammonium dimolybdate and various impurities and levels found in the prior art products of examples 1-3
Table 3 examples 1-3 and prior art products containing various impurities and amounts of high purity molybdenum trioxide
As can be seen from Table 1, the potassium content in the ammonium molybdate solutions prepared in examples 1-3 was 5ppm, 9ppm, and 8ppm, respectively, all within 10 ppm; as can be seen from table 2, the highest standard in ammonium dimolybdate at present is that the content of potassium is less than or equal to 60ppm, the content of potassium in ammonium dimolybdate produced by existing enterprises is respectively greater than 60ppm and 65ppm, while the content of potassium in ammonium dimolybdate prepared in examples 1-3 is respectively 5ppm, 8ppm and 6ppm, compared with existing products, the content of potassium is significantly reduced, mainly because the present invention performs molybdate adsorption through a plurality of ion exchange columns connected in series, while potassium ions are cations and are not adsorbed by resin, so the ammonium molybdate solution after desorption basically does not contain potassium ions. It can also be seen from table 2 that the ammonium dimolybdate prepared by the present invention has lower levels of impurities than the prior art products, except for potassium ions. As can be seen from Table 3, the potassium content of the high purity molybdenum trioxide is also significantly lower than that of the existing products.
It should be noted that, for those skilled in the art, various changes and modifications can be made without departing from the inventive concept of the present invention, and these changes and modifications belong to the protection scope of the present invention.
Claims (5)
1. A method for preparing an ammonium molybdate solution derivative product is characterized by comprising the following steps:
s1, treating the molybdenum calcine with alkali liquor to obtain a sodium molybdate solution, wherein the molybdenum calcine is low-grade molybdenum calcine; the alkali liquor is a sodium carbonate solution, and the pH value of the alkali liquor is more than 9;
s2, adsorbing the sodium molybdate solution obtained in the step S1 by an ion exchange column, wherein D314 exchange resin is selected in the ion exchange column;
s3, introducing the ammonia water solution into the ion exchange column with saturated adsorption in the step S2 for analysis to obtain the ultra-low potassium ammonium molybdate solution;
s4, carrying out evaporative crystallization on the ultra-low potassium ammonium molybdate solution obtained in the step S3 to obtain ultra-low potassium ammonium dimolybdate, and then roasting to obtain high-purity molybdenum trioxide;
and S5, sequentially introducing ammonia gas generated in the roasting process in the step S4 into a communicated primary ammonia gas absorption tower and a secondary ammonia gas absorption tower, absorbing the ammonia gas in the secondary ammonia gas absorption tower by using pure water to obtain secondary ammonia water, returning the obtained secondary ammonia water to the primary ammonia gas absorption tower for reabsorption to obtain primary ammonia water, wherein the concentration of the primary ammonia water is 3-5%, the pH value is 9-11, and finally returning the obtained primary ammonia water to an ion exchange column for analysis.
2. The method of claim 1, wherein in the step of S2, the sodium molybdate solution obtained in S1 is sequentially adsorbed by a plurality of ion exchange columns connected in series.
3. The method for preparing a derivative product of an ammonium molybdate solution according to claim 1, wherein the adsorption temperature in the step of S2 is 30 to 50 ℃.
4. An ammonium molybdate solution-derived product produced by the method of any one of claims 1 to 3, wherein the ammonium molybdate solution-derived product has a potassium content of 10ppm or less.
5. The ammonium molybdate solution derived product according to claim 4 comprising ammonium dimolybdate, ammonium tetramolybdate, ammonium heptamolybdate and high purity molybdenum trioxide.
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| CN116375087A (en) * | 2023-04-14 | 2023-07-04 | 中南大学 | A kind of preparation method of low-potassium high-purity ammonium dimolybdate |
| CN119284957B (en) * | 2024-12-11 | 2025-03-21 | 陕西恒昌钼业有限公司 | Preparation method of ultra-low potassium ammonium molybdate and ultra-low potassium derivatives thereof |
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