CN211445070U - Ammonium molybdate three-line-in-one production line - Google Patents
Ammonium molybdate three-line-in-one production line Download PDFInfo
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- CN211445070U CN211445070U CN201921797843.3U CN201921797843U CN211445070U CN 211445070 U CN211445070 U CN 211445070U CN 201921797843 U CN201921797843 U CN 201921797843U CN 211445070 U CN211445070 U CN 211445070U
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Abstract
The utility model provides a three-wire unification production line of ammonium molybdate belongs to ammonium molybdate production technical field, include: the water washing system is used for reacting the raw materials with pure water and producing a molybdenum-containing wastewater membrane concentrated solution, a low-concentration sodium molybdate solution, a primary ammonium molybdate solution and ammonia leaching residues; the acid washing system is used for treating the primary ammonium molybdate solution to obtain acid precipitation mother liquor and wet ammonium tetramolybdate; the alkaline leaching system is used for reacting low-grade molybdenum oxide, a low-concentration sodium molybdate solution, a molybdenum-containing wastewater membrane concentrated solution and caustic soda to produce a high-concentration sodium molybdate solution and alkaline leaching residues; the ion exchange system is used for carrying out adsorption and desorption treatment on the acid precipitation mother liquor and the high-concentration sodium molybdate solution to obtain a secondary ammonium molybdate solution; and the roasting system is used for drying the ammonia leaching residue and the alkaline leaching residue and carrying out roasting reaction with sodium carbonate. The utility model discloses a three-in-one production line does not have strict requirement to raw materials molybdenum oxide's grade, and the waste water that produces is low concentration ammonia nitrogen waste water, can produce calcium ammonium nitrate, realizes the zero release.
Description
Technical Field
The utility model belongs to the technical field of ammonium molybdate production, concretely relates to three-in-one production line of ammonium molybdate.
Background
Ammonium molybdate is an important link of a molybdenum processing industrial chain, and is mainly used for preparing ammonium tetramolybdate, ammonium dimolybdate, 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 production line mainly comprises: a pickling line, a water washing line and the like, wherein although the pickling line is developed to be mature, the early equipment investment is large, the unit consumption is high, and a large amount of high ammonia nitrogen wastewater is generated in the production process; the washing line has simple process, can not generate high ammonia nitrogen wastewater, but the production system has very high requirements on the grade of raw materials and impurities, limits the application range and is easy to enrich the product impurities.
SUMMERY OF THE UTILITY MODEL
Based on the above background problem, the utility model aims at providing an ammonium molybdate three-in-one production line adopts the production system that pickling line, washing line and ion exchange line combine, not only simple process, do not have the requirement to the raw materials grade, and low in production cost.
In order to achieve the above purpose, the utility model provides a technical scheme is:
an ammonium molybdate three-in-one production line comprises: the water washing system is used for reacting the raw materials with pure water and producing a molybdenum-containing wastewater membrane concentrated solution, a low-concentration sodium molybdate solution, a primary ammonium molybdate solution and ammonia leaching residues; the acid washing system is used for treating the primary ammonium molybdate solution to obtain acid precipitation mother liquor and wet ammonium tetramolybdate; the alkaline leaching system is used for reacting low-grade molybdenum oxide, a low-concentration sodium molybdate solution, a molybdenum-containing wastewater membrane concentrated solution and caustic soda to produce a high-concentration sodium molybdate solution and alkaline leaching residues; the ion exchange system is used for carrying out adsorption and desorption treatment on the acid precipitation mother liquor and the high-concentration sodium molybdate solution to obtain a secondary ammonium molybdate solution; and the roasting system is used for drying the ammonia leaching residue and the alkaline leaching residue and carrying out roasting reaction with sodium carbonate.
Wherein the molybdenum content in the acid precipitation mother liquor produced by the acid washing system is 4-8 g/L.
Wherein the content of molybdenum in the secondary ammonium molybdate solution produced by the ion exchange system is 100-140 g/L.
In one embodiment, the ammonium molybdate three-in-one production line further comprises an ammonia dissolving system, which comprises an ammonia dissolving reaction kettle for allowing the wet ammonium tetramolybdate to react with the second-level ammonium molybdate solution to obtain a third-level ammonium molybdate solution, and a crystallization device for performing evaporation crystallization on the third-level ammonium molybdate solution to obtain ammonium dimolybdate.
Wherein the molybdenum content in the tertiary ammonium molybdate solution produced in the ammonia-soluble reaction kettle is 200-250 g/L.
In one embodiment, the water washing system comprises a water washing reaction kettle for reacting raw materials, a filter for filtering materials output by the water washing reaction kettle to obtain a filter cake and filtrate, a membrane concentration device for concentrating the filtrate to obtain a molybdenum-containing wastewater membrane concentrate, and an ammonia leaching block for treating the filter cake to obtain a primary ammonium molybdate solution and ammonia leaching residues.
Wherein the content of molybdenum in the filtrate produced in the filter is 15-25g/L, the content of molybdenum in the wastewater membrane concentrated solution containing molybdenum produced in the membrane concentration equipment is 45-60g/L, and the content of molybdenum in the ammonia leaching residue is 15-25%.
In one embodiment, the alkaline leaching system comprises an alkaline leaching reaction kettle for reacting the low-concentration sodium molybdate solution, low-grade molybdenum oxide, the wastewater membrane concentrated solution and caustic soda, and a filter press for press-filtering materials output by the alkaline leaching reaction kettle to obtain the high-concentration sodium molybdate solution and alkaline leaching residues.
In one embodiment, the roasting system comprises a rotary kiln for roasting the ammonia leaching residue and the alkaline leaching residue, and a hydrolysis tank for dissolving a roasted product produced in the rotary kiln to obtain a low-concentration sodium molybdate solution.
Compared with the prior art, the utility model discloses following effect has:
1. the utility model adopts a three-in-one production line combining a pickling line, a washing line and an ion exchange line, and has no strict limitation on the grade of industrial molybdenum oxide raw materials, as long as Mo is not less than 30%; the whole production system has no chlorine ion intervention, and has low requirements on equipment materials; the wastewater is mainly low-concentration ammonia nitrogen-containing wastewater, and can be used for producing calcium ammonium nitrate to realize zero discharge.
2. The utility model discloses an ammonia among the production system soaks the sediment and soaks the sediment with alkali and dissolve molybdenum content in the filter residue and reach below 0.5%, explains and to realize through this production system that molybdenum metal conversion rate reaches more than 99.5%, increases substantially molybdenum resource utilization.
3. The production system of the utility model can control the unit consumption of ammonium molybdate per ton below 0.15 ton and the unit consumption of nitric acid below 0.5 ton.
4. The product produced by the production system of the utility model can stably reach the standard of ammonium molybdate MSA-0 product.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly described below.
FIG. 1 is a schematic structural diagram of a three-in-one production line for ammonium molybdate according to an embodiment of the present invention;
fig. 2 is a schematic flow chart of the ammonium molybdate three-in-one production line in the embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention.
In the description of the present invention, it should be noted that the terms "first level", "second level", "third level"; "first," "second," and "third" are for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In order to solve the defect that exists such as current pickling line, washing line, this embodiment provides an ammonium molybdate three-wire unification production line, includes: the water washing system is used for reacting the raw materials with pure water and producing a molybdenum-containing wastewater membrane concentrated solution, a low-concentration sodium molybdate solution, a primary ammonium molybdate solution and ammonia leaching residues; the acid washing system is used for treating the primary ammonium molybdate solution to obtain acid precipitation mother liquor and wet ammonium tetramolybdate; the alkaline leaching system is used for reacting low-grade molybdenum oxide, a low-concentration sodium molybdate solution, a molybdenum-containing wastewater membrane concentrated solution and caustic soda to produce a high-concentration sodium molybdate solution and alkaline leaching residues; the ion exchange system is used for carrying out adsorption and desorption treatment on the acid precipitation mother liquor and the high-concentration sodium molybdate solution to obtain a secondary ammonium molybdate solution; and the roasting system is used for drying the ammonia leaching residue and the alkaline leaching residue and carrying out roasting reaction with sodium carbonate.
In this embodiment, as shown in fig. 1 and 2, the water washing system includes a water washing reaction kettle 101, a first filter 102, and a membrane concentration device 103, the water washing reaction kettle 101 is used for reacting raw materials, the first filter 102 is used for filtering materials produced by the water washing reaction kettle 101 to obtain a filter cake and a filtrate, and the membrane concentration device 103 is used for concentrating the filtrate to obtain a molybdenum-containing wastewater membrane concentrate. Specifically, washing reation kettle 1 is equipped with feed inlet and discharge gate, washing reation kettle 1's discharge gate and first filter 102 intercommunication are added industrial molybdenum oxide and pure water (or filtrating) according to certain solid-to-liquid ratio from the feed inlet during the use in washing reation kettle 1, react a certain time, derive the material from the discharge gate after the reaction and filter to first filter 102 department and obtain filtrating and filter cake, and the first filter 102 of this embodiment chooses for use the belt filter to filter.
In the embodiment, the molybdenum content in the filtrate produced by the first filter 102 is 15-25g/L, the filtrate is concentrated by the membrane concentration equipment 103, the molybdenum content in the obtained membrane concentrated solution is 45-60g/L for standby, and the membrane filtrate produced by membrane concentration can be added into the water washing reaction kettle 101 to react with industrial molybdenum oxide.
In this embodiment, as shown in fig. 1, in order to treat the filter cake, the water washing system further includes an ammonia leaching block, where the ammonia leaching block includes an ammonia leaching reaction kettle 201, a second filter 202, a first rotary kiln 203, and a first hydrolysis filter tank 204, where the ammonia leaching reaction kettle 201 is configured to allow the filter cake to react with a part of ammonium molybdate solution output by the ion exchange system, the second filter 202 is configured to filter materials output by the ammonia leaching reaction kettle 201 to obtain a primary ammonium molybdate solution and ammonia leaching residues, the first rotary kiln 203 is configured to calcine the ammonia leaching residues, and the first hydrolysis filter tank 204 is configured to dissolve a roasted product output by the first rotary kiln 203 to obtain a low-concentration sodium molybdate solution. Specifically, the ammonia leaching reaction kettle 201 is provided with a feed inlet and a discharge outlet, the discharge outlet is communicated with the second filter 202, when in use, a filter cake is added into the ammonia leaching reaction kettle 201, ammonia water and a resolving solution of an ion exchange process to be described later are added into the ammonia leaching reaction kettle 201, after the reaction is finished, the second filter 202 filters the solution to obtain a primary ammonium molybdate solution and ammonia leaching residue, and the second filter 202 of the embodiment adopts a plate and frame filter press.
In this embodiment, the content of molybdenum in the ammonia leaching residue output by the second filter 202 is 15-25%, the ammonia leaching residue is dried and then added into the first rotary kiln 203 with sodium carbonate according to a certain proportion for roasting to generate solid residue containing sodium molybdate, then the solid residue is dissolved and filtered in the first hydrolysis filter tank 204 to obtain a low-concentration sodium molybdate solution for use, and the molybdenum content of the filtered residue is less than 0.5%, and the low-concentration sodium molybdate solution can be sold for sale.
In this embodiment, the acid washing system includes an acid precipitation kettle 3, a primary ammonium molybdate solution is introduced into the acid precipitation kettle 3, acid precipitation is performed to obtain an acid precipitation mother liquor and wet ammonium tetramolybdate, the molybdenum content in the acid precipitation mother liquor is 4-8g/L, and the obtained acid precipitation mother liquor enters an ion exchange system for treatment.
In this embodiment, the ion exchange system includes an ion exchange column 4, the ion exchange column 4 is filled with a weakly basic anion exchange resin d304 with a hole, the acid precipitation mother liquor is introduced into the ion exchange column 4 to adsorb molybdenum ions, the obtained filtrate is a high-concentration ammonium nitrate solution, and the resin after being analyzed can be regenerated for recycling. The ion exchange column 4 absorbed with molybdenum ions obtains a secondary ammonium molybdate solution through ammonia water resolution, wet ammonium tetramolybdate is obtained through acid precipitation treatment, the wet ammonium tetramolybdate is packaged into an ammonium tetramolybdate product after being dried for sale, and the other part of wet ammonium tetramolybdate can enter an ammonia solution block to be described later for ammonium dimolybdate production.
The ammonia dissolving block in this embodiment includes an ammonia dissolving reaction kettle 501 and a crystallization device 502, where the ammonia dissolving reaction kettle 501 is used for reacting wet ammonium tetramolybdate, specifically, the obtained wet ammonium tetramolybdate and a high-concentration ammonium molybdate solution are added into the ammonia dissolving reaction kettle 501, a secondary ammonium molybdate solution obtained by resolving the ion exchange column 4 is added into the ammonia dissolving reaction kettle 501, a tertiary ammonium molybdate solution is generated by a reaction, and the molybdenum content in the tertiary ammonium molybdate solution produced by the ammonia dissolving reaction kettle 501 is 200-250 g/L; and then introducing the tertiary ammonium molybdate solution into a crystallization device 502 for evaporation crystallization to obtain ammonium dimolybdate.
In order to recover the low-concentration sodium molybdate solution and the membrane concentrate produced in the above process, in this embodiment, the alkaline leaching system includes an alkaline leaching reactor 601 and a third filter 602, where the alkaline leaching reactor 601 is used for reacting low-grade molybdenum oxide, the low-concentration sodium molybdate solution, the molybdenum-containing wastewater membrane concentrate with caustic soda, and the third filter 602 is used for performing filter pressing on the material produced by the alkaline leaching reactor 601 to obtain a high-concentration sodium molybdate solution and alkaline leaching residues, the obtained alkaline leaching residues are calcined in a second rotary kiln 603, and the calcined product enters a second hydrolysis filter tank 604 to be dissolved to obtain the low-concentration sodium molybdate solution. Specifically, adding low-grade molybdenum oxide, alkali liquor, a low-concentration sodium molybdate solution and a molybdenum-containing wastewater membrane concentrated solution into an alkaline leaching reaction kettle 601 according to a certain solid-to-liquid ratio, after reacting for a period of time, introducing the materials into a third filter 602 for filter pressing to obtain a high-concentration sodium molybdate solution and alkaline leaching residues, drying the alkaline leaching residues and the ammonia leaching residues, adding the dried alkaline leaching residues and sodium carbonate into a second rotary kiln 603 according to a certain proportion for roasting to generate solid residues containing sodium molybdate, dissolving and filtering the solid residues in a second hydrolysis filter tank 604 to obtain a low-concentration sodium molybdate solution for later use, wherein the molybdenum content of the filtered filter residues is less than 0.5%, and the filter residues can be sold for external use; the low-concentration sodium molybdate solution can be returned to the alkaline leaching reaction kettle 601 for recycling.
The high-concentration sodium molybdate solution produced in the alkaline leaching process is treated by an ion exchange system, namely the high-concentration sodium molybdate solution is introduced into an ion exchange column 4 to adsorb molybdate ions, and then a secondary ammonium molybdate solution is obtained by ammonia water analysis, wherein the molybdenum content in the obtained secondary ammonium molybdate solution is 100-140 g/L. Namely, the ion exchange system of this embodiment is provided with two sets of ion exchange columns, one set of ion exchange columns is used for adsorption and desorption treatment of the acid precipitation mother liquor, and the other set of ion exchange columns is used for adsorption and desorption treatment of the high-concentration sodium molybdate solution.
In each of the above systems, the following reaction principles are involved:
(1) the chemical equation for the reaction in the water washing reaction kettle 101 is:
MoO3+H2O→H2MoO4
(2) the chemical equation for the reaction in the ammonia leaching reaction kettle 201 is as follows:
H2MoO4+2NH4OH→(NH4)2MoO4+2H2O
(3) the chemical equation for the reaction in the first rotary kiln 203 is:
Na2CO3+H2MoO4→Na2MoO4+H2O+CO2
(4) the chemical equation for the reaction in the acid precipitation tank 3 is:
4(NH4)2MoO4+6HNO3→(NH4)2Mo4O13↓+6NH4NO3+3H2O
(5) the chemical equation for the reaction in the crystallization apparatus 502 is:
2(NH4)2Mo O4→(NH4)2Mo2O7+2NH3+H2O
it should be noted that, the filtering apparatus in this embodiment includes the first filter 102, the second filter 202 and the third filter 602, and in specific use, only one filter may be used for processing related processes; the roasting equipment comprises a first rotary kiln 203 and a second rotary kiln 603, and in specific use, only one rotary kiln can be used for treatment.
It should be noted that, the number of the ion exchange columns 4 in the ion exchange system can be plural in series according to the requirement, and the present invention is not limited specifically.
It should be noted that, for those skilled in the art, without departing from the inventive concept, several variations and modifications can be made, which are within the scope of the present invention.
Claims (5)
1. The utility model provides an ammonium molybdate three-in-one production line which characterized in that includes:
the water washing system is used for reacting the raw materials with pure water and producing a molybdenum-containing wastewater membrane concentrated solution, a low-concentration sodium molybdate solution, a primary ammonium molybdate solution and ammonia leaching residues;
the acid washing system is used for treating the primary ammonium molybdate solution to obtain acid precipitation mother liquor and wet ammonium tetramolybdate;
the alkaline leaching system is used for reacting low-grade molybdenum oxide, a low-concentration sodium molybdate solution, a molybdenum-containing wastewater membrane concentrated solution and caustic soda to produce a high-concentration sodium molybdate solution and alkaline leaching residues;
the ion exchange system is used for carrying out adsorption and desorption treatment on the acid precipitation mother liquor and the high-concentration sodium molybdate solution to obtain a secondary ammonium molybdate solution;
and the roasting system is used for drying the ammonia leaching residue and the alkaline leaching residue and carrying out roasting reaction with sodium carbonate.
2. The ammonium molybdate three-in-one production line according to claim 1, further comprising an ammonia dissolving system, which comprises an ammonia dissolving reaction kettle for reacting the wet ammonium tetramolybdate with the second ammonium molybdate solution to obtain a third ammonium molybdate solution, and a crystallization device for performing evaporative crystallization on the third ammonium molybdate solution to obtain ammonium dimolybdate.
3. The ammonium molybdate three-in-one production line as claimed in claim 1, wherein the water washing system comprises a water washing reaction kettle for raw material reaction, a filter for filtering materials produced by the water washing reaction kettle to obtain a filter cake and filtrate, a membrane concentration device for concentrating the filtrate to obtain a molybdenum-containing wastewater membrane concentrate, and an ammonia leaching block for treating the filter cake to obtain a primary ammonium molybdate solution and ammonia leaching residues.
4. The ammonium molybdate three-in-one production line according to claim 1, wherein the alkaline leaching system comprises an alkaline leaching reaction kettle for reacting the low-concentration sodium molybdate solution, the low-grade molybdenum oxide, the wastewater membrane concentrated solution and caustic soda, and a filter press for press-filtering materials output by the alkaline leaching reaction kettle to obtain the high-concentration sodium molybdate solution and alkaline leaching residues.
5. The ammonium molybdate three-in-one production line as claimed in claim 1, wherein the roasting system comprises a rotary kiln for roasting the ammonia leaching residue and the alkaline leaching residue, and a hydrolysis tank for dissolving a roasted product produced in the rotary kiln to obtain a low-concentration sodium molybdate solution.
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| CN115464415A (en) * | 2022-09-26 | 2022-12-13 | 荆大（荆州）汽车配件有限公司 | Three-in-one automobile pipe production system and method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115464415A (en) * | 2022-09-26 | 2022-12-13 | 荆大（荆州）汽车配件有限公司 | Three-in-one automobile pipe production system and method |
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