CN110937634B - Production method for preparing ammonium molybdate by calcium molybdate raw material ammonium phosphate mixed liquid transformation method - Google Patents
Production method for preparing ammonium molybdate by calcium molybdate raw material ammonium phosphate mixed liquid transformation method Download PDFInfo
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Abstract
The invention discloses a production method for preparing ammonium molybdate by a calcium molybdate raw material ammonium phosphate mixed solution transformation method, which comprises the following steps: s1, mixing the calcium molybdate raw material with transformation mother liquor containing ammonium phosphate to obtain primary transformation slag and primary transformation mother liquor; s2, processing the primary transformation slag for multiple times by using an ammonium phosphate solution to obtain transformation mother liquor containing ammonium phosphate and final transformation slag, wherein the transformation mother liquor is used as a raw material mixed by transformation slag and/or calcium molybdate raw materials; s3, mixing the primary transformation mother liquor with ammonium sulfide, and then filtering the transformation mother liquor; s4, adding cations which are precipitated with phosphate ions into the transformation mother liquor, and filtering the transformation mother liquor; and S5, carrying out evaporative crystallization treatment on the rotary mold mother liquor to obtain a crystal. The invention solves the problems of difficult control of the process, difficult filtration of particles, easy corrosion of equipment and the like in the prior ammonium molybdate preparation method by acid decomposition ammonia dissolution by adopting a mode of more environmental protection, high efficiency and low cost.
Description
Technical Field
The invention relates to the technical field of ammonium molybdate production, in particular to a production method for preparing ammonium molybdate by a calcium molybdate raw material ammonium phosphate mixed solution transformation method.
Background
In recent years, in the recovery treatment of molybdenum waste liquid in the industry, a method of directly adding calcium salt into waste water is partially adopted, and a process for producing calcium molybdate through liquid-phase precipitation is adopted, so that some recovered products of calcium molybdate are produced. At present, the main treatment ideas for calcium molybdate include the following:
(1) preparing ammonium molybdate by an acid decomposition ammonia dissolution method: calcium molybdate-acid decomposition-molybdic acid filter cake-ammonia water dissolution-crude ammonium molybdate solution-magnesium chloride impurity removal-ammonia sulfide impurity removal-refined ammonium molybdate solution-nitric acid precipitation-ammonium tetramolybdate-ammonia dissolution-evaporative crystallization-ammonium dimolybdate;
(2) preparing sodium molybdate by using a sodium carbonate high-pressure leaching method: calcium molybdate-sodium carbonate leaching-sodium molybdate solution-evaporative crystallization-sodium molybdate solid;
(3) and preparing molybdenum alloy or molybdenum metal by high-temperature reduction: calcium molybdate-high temperature reduction-molybdenum alloy or molybdenum metal.
For preparing ammonium molybdate by acid decomposition ammonia dissolution method, the method is a common recovery method for hydrometallurgy, because the ammonium molybdate product with higher value can be prepared, but the method has the following defects: (1) the process is not easy to control during acid decomposition, and molybdic acid particles are fine and difficult to filter. (2) The working environment is poor, and the equipment is easy to corrode; (3) the automatic control is not easy to be realized; (4) environmental emission (such as waste water, waste gas, waste residue and the like) is difficult to meet the national requirements, ammonia nitrogen compounds with high concentration are generated due to large ammonia consumption of ammonia leaching in the production process, the ammonia nitrogen in the waste water emission seriously exceeds the standard, the treatment of ammonia nitrogen waste needs to be solved at a great cost, and the process faces serious challenges.
For the sodium molybdate prepared by the sodium carbonate high-pressure leaching method, the sodium molybdate leaching method is used by part of domestic manufacturers and has the following defects: (1) the equipment requirement is high, the operation must be carried out under high pressure, otherwise, the utilization coefficient of the sodium carbonate is low; (2) the sodium molybdate product has low value, and the same metal amount is discounted compared with the price of raw ore. Resulting in a high cost of the method.
For molybdenum alloy or molybdenum metal prepared by high-temperature reduction, the following defects exist in part ferromolybdenum manufacturers: the applicability to raw materials is very poor, and in particular, ferromolybdenum produced when the original calcium molybdate P and S elements are relatively high is difficult to use by iron and steel enterprises.
Disclosure of Invention
The invention aims to: aiming at the problems, the production method for preparing ammonium molybdate by the calcium molybdate raw material ammonium phosphate mixed solution transformation method is provided, and the problems of difficult process control, difficult particle filtration, easy equipment corrosion and the like in the existing ammonium molybdate preparation method by acid decomposition ammonia dissolution are solved by adopting a more environment-friendly, efficient and low-cost mode.
The technical scheme adopted by the invention is as follows: the production method for preparing ammonium molybdate by using a calcium molybdate raw material ammonium phosphate mixed solution transformation method is characterized by comprising the following steps of:
s1, mixing the calcium molybdate raw material with transformation mother liquor containing ammonium phosphate, and filtering after reaction to obtain primary transformation slag and primary transformation mother liquor;
s2, adding water into ammonium phosphate raw materials (such as monoammonium phosphate, diammonium phosphate and triammonium phosphate) and ammonia water to prepare an ammonium phosphate solution, treating the primary transformation slag for multiple times by the ammonium phosphate solution to obtain transformation mother liquor containing the ammonium phosphate and final transformation slag, using the transformation mother liquor containing the ammonium phosphate as a raw material for mixing transformation slag and/or calcium molybdate raw materials, and using the final transformation slag as waste slag to enter a waste slag treatment process;
s3, mixing the primary transformation mother liquor with a designed amount of ammonium sulfide, and then filtering the transformation mother liquor;
s4, adding cations which generate precipitates with phosphate ions into the transformation mother liquor obtained in the S3, mixing and reacting, and filtering the transformation mother liquor;
s5, carrying out evaporation crystallization treatment on the transformation mother liquor obtained in the S4 to obtain a crystal, and drying the crystal to obtain an ammonium molybdate product.
In the method, ammonium phosphate is used as mother liquor to prepare raw materials, the obtained ammonium phosphate solution belongs to neutral solution and does not corrode equipment, the equipment only uses common stainless steel materials, the calcium molybdate raw materials are dissolved by the ammonium phosphate solution to form calcium phosphate precipitate and ammonium molybdate, crude ammonium molybdate solution (namely primary conversion mother liquor) is obtained after filtration, then ammonium sulfide is added to remove impurities, high carbon ammonium molybdate solution containing a certain amount of phosphate ions is obtained after filtration, then cations which generate precipitates with the phosphate ions, such as magnesium chloride, calcium chloride, ferric chloride and other water-soluble inorganic salts are added to introduce the cations to remove the phosphate ions in the conversion mother liquor, the trace excess cations can be removed by using a resin ion exchange column to obtain high purity ammonium molybdate solution, and finally the high purity ammonium molybdate solution is subjected to evaporation crystallization treatment, and further obtaining high-purity crystals, and drying the crystals to obtain the high-purity ammonium molybdate product. Furthermore, in the invention, the transformation slag is treated for a plurality of times and the treated transformation mother liquor is recycled, mainly in order to improve the recovery rate of ammonium molybdate, the transformation slag obtained after the calcium molybdate is primarily transformed contains more calcium molybdate which is not transformed, the recovery rate is lower, the molybdenum resource waste is serious, and the process requirement of enterprises cannot be met, and after the transformation slag and the transformation mother liquor are fully recycled, the recovery rate of the molybdenum resource is improved, the transformation mother liquor is fully utilized, the raw material cost is greatly reduced, the waste liquor generation amount is small, and the transformation mother liquor in the intermediate process can be directly utilized, so that the effect of high-efficiency transformation production is achieved, and the production of high recovery rate, environmental protection, high efficiency and low cost of ammonium molybdate is finally ensured.
Compared with the traditional process for preparing ammonium molybdate by an ammonia dissolving method through acid decomposition, the method has the advantages that: (1) the method of the invention takes ammonium phosphate solution as mother liquor, the reaction process is stable and easy to control, and the ammonium molybdate is extracted by adopting an evaporation crystallization mode, so that the problem that the ammonium molybdate is fine and difficult to filter does not exist; (2) the solution used for producing ammonium molybdate is neutral or slightly alkaline, the corrosion capability to equipment is extremely low, acid and alkali resistant equipment such as titanium alloy and the like is not needed, and the equipment investment cost is low; (3) the method of the invention is easy to realize automatic production, simple and reliable to control and high in production efficiency.
Further, compared with the method for preparing ammonium molybdate by using a calcium molybdate raw material ammonium bicarbonate mixed liquid transformation method, which is another patent application of the inventor, the method has the advantages that: the ammonium phosphate is used for preparing the ammonium molybdate, the conversion rate of the raw material calcium molybdate is higher than that of the ammonium carbonate for preparing the ammonium molybdate, but the use cost of the ammonium phosphate is higher than that of the ammonium carbonate, phosphorus needs to be removed again in the later process of preparing the ammonium phosphate, the process is troublesome, and carbon can be removed only by blowing off and recycling in the later process of preparing the ammonium carbonate, so that the method is simple and convenient.
Preferably, in S2, the primary transformation slag is mixed with the tertiary transformation mother liquor, and then filtered to obtain a secondary transformation mother liquor and a secondary transformation slag, the secondary transformation mother liquor is used for mixing with the calcium molybdate raw material, the secondary transformation slag is mixed with the prepared ammonium phosphate solution, and after filtering, a tertiary transformation mother liquor and a tertiary transformation slag are obtained, the tertiary transformation liquor is used for mixing with the primary transformation slag, and the tertiary transformation slag is treated as the final transformation slag. According to the preferred scheme, the calcium molybdate raw material is treated by the secondary transformation mother liquor, the tertiary transformation mother liquor is mixed with the ammonium phosphate solution to supplement ammonium in the mother liquor, then molybdenum resources in the transformation slag are recovered by the tertiary transformation mother liquor and the secondary transformation mother liquor, and the ammonium phosphate raw material is fully utilized while the recovery rate is improved. Of course, the number of transformation of the transformation mother liquor can be adjusted according to the actual raw material conditions, and is not limited to 3 transformation treatments.
In the invention, in order to obtain ammonium molybdate through crystallization, simultaneously recycle ammonium in the transformation mother liquor and achieve the effect of zero emission of ammonia nitrogen, when evaporation crystallization treatment is carried out, gas generated in the treatment process is absorbed by an absorption tower, and absorption liquid is used for preparing ammonium phosphate solution.
Further, the ammonium phosphate raw material and ammonia water are added with water to prepare an ammonium phosphate solution, the phosphorus concentration of phosphate ions is 5-25g/L, and the concentration of free ammonium hydroxide is 10-30 g/L.
Further, the solid-liquid mass ratio of the calcium molybdate raw material to the transformation mother liquor is 1: (1-20), when the transformation slag and the transformation mother liquor are mixed, the solid-liquid mass ratio of the transformation slag to the transformation mother liquor is 1: (1-20).
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
1. compared with the traditional process for preparing ammonium molybdate by acid decomposition ammonia dissolution, the method has the advantages that the acid decomposition process is not adopted, so that the acid decomposition process is avoided, the method takes ammonium phosphate solution as mother liquor, the reaction process is stable and easy to control, the ammonium molybdate is extracted by adopting an evaporation crystallization mode, and the problem that the ammonium molybdate is fine in particles and difficult to filter is avoided; the solution used for producing ammonium molybdate is a neutral solution, the corrosion capability to equipment is extremely low, the method is easy to realize automatic production, the control is simple and reliable, and the production efficiency is high;
2. the invention realizes the production effect of zero emission of ammonia nitrogen, solves the problems of serious excessive ammonia nitrogen in the wastewater and high cost treatment of the wastewater, greatly reduces the environmental protection pressure of enterprises, and improves the profit margin of the enterprises;
3. the method has the advantages of high recovery rate, high ammonium molybdate yield, high efficiency, stability and easy automation control, and each index of the ammonium molybdate product meets the highest standard of the national standard, thereby being worthy of application and popularization.
Drawings
FIG. 1 is a schematic process flow diagram of a production method for preparing ammonium molybdate by a calcium molybdate raw material ammonium phosphate mixed liquid transformation method.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings.
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
As shown in fig. 1, a production method for preparing ammonium molybdate by a calcium molybdate raw material ammonium phosphate mixed solution transformation method comprises the following steps:
s1, mixing the calcium molybdate raw material with the secondary transformation mother liquor according to the solid-liquid mass ratio of 1: (1-20) mixing, controlling the mixing reaction temperature at 20-80 ℃ for 0.5-6 h, and performing pressure filtration by a filter press after reaction to obtain primary transformation slag (namely primary transformation slag) and primary transformation mother liquor;
s2, adding water into ammonium phosphate raw materials (such as monoammonium phosphate, diammonium phosphate and triammonium phosphate) and ammonia water to prepare an ammonium phosphate solution, wherein the phosphorus concentration of phosphate ions is 5-25g/L, the free ammonium hydroxide concentration is 10-30g/L, and the solid-liquid mass ratio of the primary transformation slag to the tertiary transformation mother solution is 1: (1-20), controlling the mixing reaction temperature at 20-80 ℃ for 0.5-6 h, then performing pressure filtration by a filter press to obtain secondary transformation mother liquor and secondary transformation slag, returning the secondary transformation mother liquor to be continuously mixed with the calcium molybdate raw material, and mixing the secondary transformation slag with the prepared ammonium phosphate solution according to the solid-liquid mass ratio of 1: (1-20), controlling the mixing reaction temperature at 20-80 ℃ for 0.5-6 h, and performing pressure filtration by a pressure filter to obtain a tertiary transformation liquid and tertiary transformation slag, wherein the tertiary transformation mother liquid is used for mixing with the primary transformation slag, and the tertiary transformation slag is treated as final waste slag after being subjected to pressure filtration and blow drying;
s3, mixing the primary transformation mother liquor with a designed amount of ammonium sulfide, and then filtering the transformation mother liquor;
s4, adding cations such as magnesium chloride which can generate precipitates with phosphate ions into the transformation mother liquor obtained in S3, mixing and reacting, and filtering the transformation mother liquor;
and S5, carrying out evaporation crystallization treatment on the transformation mother liquor obtained in the step S4 to obtain a crystal, and drying the crystal to obtain an ammonium molybdate product.
In the invention, in order to obtain ammonium molybdate through crystallization, simultaneously recycle ammonium in the transformation mother liquor and achieve the effect of zero emission of ammonia nitrogen, when evaporation crystallization treatment is carried out, gas generated in the treatment process is absorbed by an absorption tower, namely cold water in the absorption tower is absorbed to form ammonia water absorption liquid, and the ammonia water absorption liquid is used for preparing ammonium phosphate solution.
In order to better explain the invention, specific examples are listed below:
example 1
Preparing a new liquid: 300Kg of ammonium phosphate is used, and 1.5-2 m of ammonium phosphate is added 3 Tap water, then ammonia water 0.3-0.4 m of 10-15% absorbed by the back section 3 Stirring for about half an hour to prepare a new conversion solution;
(II) transformation reaction: the raw material calcium molybdate containing 46 percent (mass fraction) of molybdenum is 150-200 Kg, and 1.5-2 m of calcium molybdate is added 3 Heating the secondary transformation mother liquor to 40-50 deg.C for 2 hr, filtering with filter press to obtain primary transformation mother liquor and primary transformation slag, removing impurities from the primary transformation mother liquor, and mixing the primary transformation slag with 1.5-2 m 3 Reacting the third transformation mother liquor at 40-50 deg.C for 2 hr to obtain second transformation residue and second transformation mother liquor, returning the second transformation mother liquor to use, and reacting the second transformation residue with 1.5-2 m 3 The transformation new liquid reacts to obtain three transformation slags, and the transformation slags are obtained by measurement, wherein the molybdenum content in the three transformation slags is less than or equal to 1 percent, and the slag rate is about 52 percentThe comprehensive molybdenum recovery rate reaches 98.9 percent;
(III) removing impurities with reagent, using ammonium sulfide solution 0.05-0.1 m 3 Adding into primary transformation mother liquor, stirring for 1 hr, clarifying, filtering, and adding into the clear liquid for 0.1m 3 Adding 27% hydrogen peroxide into the primary transformation liquid, and stirring for 1 hour;
removing impurities with reagent II, preparing magnesium chloride into 50-150 g/L solution, and adding 0.05-0.1 m 3 Adding the magnesium chloride solution into the clear liquid added with hydrogen peroxide in the previous step, stirring for 1 hour, then clarifying and filtering to obtain clear liquid, and removing a small amount of cations from the clear liquid through chelating resin to obtain pure ammonium molybdate solution;
and (V) evaporating and filtering the obtained ammonium molybdate solution, drying crystals after crystallization to obtain an ammonium dimolybdate product, and recycling ammonia gas generated in the process to prepare a new conversion solution again.
Example 2
Preparing a new liquid: 300Kg of diammonium phosphate is used, and 1.5-2 m of diammonium phosphate is added 3 Adding tap water, and adding 0.3-0.4 m of 10-15% ammonia water absorbed by the back section 3 Stirring for about half an hour to prepare a new conversion solution;
(II) transformation reaction: the raw material calcium molybdate containing 45 percent of molybdenum is 150-200 Kg, and 1.5-2 m of calcium molybdate is added 3 Heating the secondary transformation mother liquor to 40-50 deg.C for 2 hr, filtering with filter press to obtain primary transformation mother liquor and primary transformation slag, removing impurities from the primary transformation mother liquor, and mixing the primary transformation slag with 1.5-2 m 3 Reacting the third transformation mother liquor at 40-50 deg.C for 2 hr to obtain second transformation residue and second transformation mother liquor, returning the second transformation mother liquor to use, and reacting the second transformation residue with 1.5-2 m 3 Carrying out a reaction on the transformation new liquid to obtain three transformation slags, and measuring to obtain the transformation slag, wherein the molybdenum content of the three transformation slags is less than or equal to 1.5%, the slag rate is about 54%, and the comprehensive molybdenum recovery rate reaches 98.2%;
(III) removing impurities with reagent, using ammonium sulfide solution 0.05-0.1 m 3 Adding into primary transformation mother liquor, stirring for 1 hr, clarifying, filtering, and adding into the clear liquid for 0.1m 3 27% strengthAdding hydrogen peroxide of certain degree into the primary transformation liquid, and stirring for 1 hour;
(IV) removing impurities with a reagent II, preparing magnesium sulfate into a solution of 50-150 g/L, and then adding 0.05-0.1 m 3 Adding the magnesium chloride solution into the clear liquid added with hydrogen peroxide in the previous step, stirring for 1 hour, then clarifying and filtering to obtain clear liquid, and removing a small amount of cations from the clear liquid through chelating resin to obtain pure ammonium molybdate solution;
and (V) evaporating and filtering the obtained ammonium molybdate solution, drying crystals after crystallization to obtain an ammonium dimolybdate product, and recycling ammonia gas generated in the process to prepare a new conversion solution again.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (5)
1. The production method for preparing ammonium molybdate by using a calcium molybdate raw material ammonium phosphate mixed solution transformation method is characterized by comprising the following steps of:
s1, mixing the calcium molybdate raw material with transformation mother liquor containing ammonium phosphate, and filtering after reaction to obtain primary transformation slag and primary transformation mother liquor;
s2, adding water into the ammonium phosphate raw material and ammonia water to prepare an ammonium phosphate solution, processing the primary transformation slag for multiple times by the ammonium phosphate solution to obtain transformation mother liquor containing the ammonium phosphate and final transformation slag, using the transformation mother liquor containing the ammonium phosphate as a raw material for mixing transformation slag and/or calcium molybdate raw materials, and using the final transformation slag as waste slag to enter a waste slag treatment process;
s3, mixing the primary transformation mother liquor with a designed amount of ammonium sulfide, and then filtering the transformation mother liquor;
s4, adding cations which generate precipitates with phosphate ions into the transformation mother liquor obtained in the S3, mixing and reacting, and filtering the transformation mother liquor;
and S5, carrying out evaporation crystallization treatment on the transformation mother liquor obtained in the step S4 to obtain a crystal, and drying the crystal to obtain an ammonium molybdate product.
2. The method for producing ammonium molybdate according to claim 1, wherein in step S2, the primary transformation slag is mixed with the tertiary transformation mother liquor, and then filtered to obtain a secondary transformation mother liquor and a secondary transformation slag, the secondary transformation mother liquor is used for mixing with the calcium molybdate raw material, the secondary transformation slag is mixed with the prepared ammonium phosphate solution, and after filtering, the tertiary transformation mother liquor and the tertiary transformation slag are obtained, the tertiary transformation mother liquor is used for mixing with the primary transformation slag, and the tertiary transformation slag is treated as the final transformation slag.
3. The method for producing ammonium molybdate according to claim 1, wherein the absorption liquid is used for preparing ammonium phosphate solution after the gas generated in the process is absorbed by the absorption tower during the evaporation and crystallization process.
4. The method for producing ammonium molybdate according to claim 1, wherein the ammonium phosphate raw material and the ammonia water are added with water to prepare an ammonium phosphate solution, the phosphorus concentration of phosphate ions is 5-25g/L, and the concentration of free ammonium hydroxide is 10-30 g/L.
5. The method for producing ammonium molybdate by the calcium molybdate raw material ammonium phosphate mixed liquor conversion method as claimed in claim 2, wherein the solid-liquid mass ratio of the calcium molybdate raw material to the conversion mother liquor is 1: (1-20), when the transformation slag and the transformation mother liquor are mixed, the solid-liquid mass ratio of the transformation slag to the transformation mother liquor is 1: (1-20).
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| CN106435178A (en) * | 2016-11-25 | 2017-02-22 | 桂林理工大学 | Method for decomposing oxidized ore of molybdenum through ordinary pressure alkali |
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Inventor after: Liu Yang Inventor after: Liu Jinrui Inventor after: Yang Wei Inventor after: Gao Zhiqiang Inventor after: Zheng Zhimu Inventor before: Liu Jinrui Inventor before: Liu Yang Inventor before: Yang Wei Inventor before: Gao Zhiqiang Inventor before: Zheng Zhimu |