CN108083335A - The technique that a kind of ion-exchange produces high-purity ammonium dimolybdate - Google Patents
The technique that a kind of ion-exchange produces high-purity ammonium dimolybdate Download PDFInfo
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- CN108083335A CN108083335A CN201810083347.5A CN201810083347A CN108083335A CN 108083335 A CN108083335 A CN 108083335A CN 201810083347 A CN201810083347 A CN 201810083347A CN 108083335 A CN108083335 A CN 108083335A
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Abstract
The invention discloses the techniques that a kind of ion-exchange produces high-purity ammonium dimolybdate, comprise the following steps：First, prepared by sodium molybdate solution：(1) dissolving, (two) filtering and secondary leaching；2nd, ion exchange：(1) absorption, (two) parsing；3rd, crystallize and dry.Ion-exchange of the present invention produces ammonium molybdate, not only with environment-friendly advantage, realizes ammonia nitrogen and recycles on stream, meets the technological requirement of clean manufacturing；And short flow, good impurity removing effect, controlled process degree is high, product with stable quality；Required auxiliary material less varieties, ion exchange resin can Reusability, material movement is few；Automation control is easily carried out, is conducive to labor intensity of raising labour productivity and reduce, working environment is good, there is preferable social benefit；Adaptability to raw material is strong, and metal recovery rate is high, can handle various low-grade calcinings and various other raw materials containing molybdenum.
Description
Technical field
The invention belongs to chemical technology field, more particularly to a kind of work of the high-purity ammonium dimolybdate of ion-exchange production
Skill.
Background technology
The raw material of conventional production of molybdic ammonium is molybdenite, and production work technique is：Molybdenite --- roasting --- industrial oxygen
Change molybdenum --- pickling --- ammonia leaching --- thick ammonium molybdate solution --- magnesium chloride removal of impurities --- vulcanization ammonia removal of impurities --- smart ammonium molybdate
Solution --- nitric acid acid is heavy --- ammonium tetramolybdate --- ammonia is molten --- evaporative crystallization --- ammonium dimolybdate.Classical approach produces ammonium molybdate
Process flow chart is as shown in Figure 1.
The method of classical approach production ammonium molybdate is that China applies wider method at present, feature be equipment is simple, investment compared with
It is small, treating capacity is small, but the method has the following disadvantages：(1) industrial oxidation molybdenum leaching rate is not high when ammonia soaks, and molybdenum is in the art in slag
It is not easily recycled, causes the rate of recovery low, it is of high cost；(2) impurity-eliminating effect is poor, and product chemical property is relatively inaccessible to national standard；(3)
Adaptability to raw material is poor, and the molybdenum concntrate that quality can only be used higher can be only achieved national standard for raw produce；(4) working environment
Difference, equipment are perishable；(5) it is not easy to carry out automation control；(6) environment protection emission (such as waste water, exhaust gas and waste residue) is difficult to reach
National requirements, since ammonia soaks a large amount of consumption ammonia in production process, the heavy a large amount of consumption nitric acid of acid generate the ammonia nitrogen chemical combination of a large amount of high concentrations
Object causes discharge of wastewater ammonia nitrogen to severely exceed, and very big cost must be spent to solve the improvement of ammonia nitrogen waste, this is the life of classical approach technique
Maximum disadvantage caused by production.Present China environmental pollution pay attention to day by day, classical approach production technology are faced with stern challenge,
And the process route of ion-exchange production ammonium molybdate has stronger advantage in production of molybdic ammonium is solved in terms of ammonia nitrogen improvement,
Three waste discharge can reach national discharge index.
The content of the invention
Goal of the invention：The defects of overcoming traditional production of molybdic ammonium industrial for the molybdenum raw material of various complexity, provides one kind
Distinctive ion-exchange produces the technique of high-purity ammonium dimolybdate, and environmental protection and energy saving, wide adaptability, are easy to automate short flow
Control, product ammonium dimolybdate stable quality, indices meet national standard highest standard.
Technical solution：A kind of ion-exchange produces the technique of high-purity ammonium dimolybdate, comprises the following steps：
First, prepared by sodium molybdate solution：(1) dissolving, (two) filtering and secondary leaching；2nd, ion exchange：(1) adsorb,
(2) parse；3rd, crystallize and dry.
It is as follows：
First, prepared by sodium molybdate solution
(1) dissolve：
By molybdenum raw material (industrial molybdenum trioxide, molybdenum dioxide, molybdenum sulfide, molybdate any of which or a variety of mixtures)
With NaOH solution with molybdenum alkali molar ratio 1 in dissolving tank:1~1:2 ratio mixing, in 70~100 DEG C of temperature, solid-to-liquid ratio 1:5
~1：When reaction 2~3 is small under conditions of 10, thick sodium molybdate slurry, a part of solvable molybdenum and caustic soda reaction generation sodium molybdate is made
Solution is stored in, the molybdate compounds such as the undissolved molybdenum dioxide of another part, molybdenum sulfide and molybdate then stay in slag phase；
(2) filtering and secondary leaching：
Thick sodium molybdate slurry is obtained after dissolving to filter by filter press, obtains clear liquid and primary slag；Clear liquid is thick sodium molybdate
Solution；In the primary slag of different material containing molybdenum between 5%~20%；The primary slag of leaching is according to solid-to-liquid ratio 1:3~1:5th, alkali
It spends 50~200g/l and carries out slurrying, soaked using secondary alkali, reaction condition is：200~220 DEG C of temperature, partial pressure of oxygen 1.5~
2.0MPa, reaction time：2 it is small when, the leaching of secondary alkali make in primary slag 98.5%~99.5% molybdenum also in the form of sodium molybdate into
Enter liquid phase, the filtrate that two level press filtration generates returns to dissolving step and utilizes.
2nd, ion exchange
(1) adsorb
Sodium molybdate solution through dissolving and being obtained by filtration, by adding water that feed liquid molybdenum concentration (mass concentration of Mo elements) is dilute
It releases to 10~40g/l, solution is with 5~30m after dilution3The flow of/h is by a kind of anion exchange resin, and molybdenum is with more molybdates
Form be adsorbed onto on resin；Using the resin of clear water washing adsorption saturation, the more molybdates adsorbed on resin also on resin,
It washes away simultaneously remaining containing molybdenum solution in ion exchange column, impurity interference is just avoided that when parsing in next step；Wash water returns thick
Sodium molybdate dilution step；
(2) parse
With saturated ammonium chloride solution (NH4Cl) as parsing agent, with 2.5~15m3The flow velocity of/h to adsorption saturation it is cloudy from
Sub-exchange resin is eluted, parsed, and the more molybdates adsorbed on resin return to solution, is formed ammonium molybdate with ammonia, is obtained
The pure ammonium molybdate solution of 120~180g/l of molybdenum concentration；Resin is washed with clear water, since the molybdate on resin is replaced
Afterwards, saturated ammonium chloride solution is also remained in ion exchange column, this moieties is come out, to carry out the absorption of next round
Operation.
3rd, crystallize and dry
Pure ammonium molybdate solution obtains ammonium dimolybdate by crystallization, through vacuum filter, using being packaged to be after microwave drying
High-purity ammonium dimolybdate finished product；
The ammonia generated with the absorption by Hydrochloric Acid crystallization process of Wt30%, is made ammonium chloride solution, returns to ion-exchange process
For parsing, recycled so as to fulfill ammonia nitrogen, ammonia nitrogen zero-emission.
Beneficial effects of the present invention：Ion-exchange of the present invention produces ammonium molybdate, not only with environment-friendly advantage, realizes ammonia
Nitrogen recycles on stream, meets the technological requirement of clean manufacturing；And short flow, good impurity removing effect, controlled process degree
Height, product with stable quality；Required auxiliary material less varieties, ion exchange resin can Reusability, material movement is few；It easily carries out certainly
Dynamicization controls, and is conducive to labor intensity of raising labour productivity and reduce, working environment is good, there is preferable social benefit；Raw material
Adaptable, metal recovery rate is high, can handle various low-grade calcinings (high tungsten, high-copper, high lead, high silicon) and various other contain
Molybdenum raw material.
Description of the drawings
Fig. 1 is classical approach production ammonium molybdate process flow diagram；
Fig. 2 is ion-exchange production ammonium molybdate process flow chart of the present invention.
Specific embodiment
It is right in the following with reference to the drawings and specific embodiments in order to make the object, technical solutions and advantages of the present invention clearer
The present invention is described in detail.
First, prepared by sodium molybdate solution
(1) dissolve：
By molybdenum raw material (industrial molybdenum trioxide, molybdenum dioxide, molybdenum sulfide, molybdate any of which or a variety of mixtures)
With NaOH solution with molybdenum alkali molar ratio 1 in dissolving tank:1~1:2 ratio mixing, in 70~100 DEG C of temperature, solid-to-liquid ratio 1:5
~1：When reaction 2~3 is small under conditions of 10, thick sodium molybdate slurry, a part of solvable molybdenum and caustic soda reaction generation sodium molybdate is made
Solution is stored in, the molybdate compounds such as the undissolved molybdenum dioxide of another part, molybdenum sulfide and molybdate then stay in slag phase；
(2) filtering and secondary leaching：
Thick sodium molybdate slurry is obtained after dissolving to filter by filter press, obtains clear liquid and primary slag；Clear liquid is thick sodium molybdate
Solution；In the primary slag of different material containing molybdenum between 5%~20%；The primary slag of leaching is according to solid-to-liquid ratio 1:3~1:5th, alkali
It spends 50~200g/l and carries out slurrying, soaked using secondary alkali, reaction condition is：200~220 DEG C of temperature, partial pressure of oxygen 1.5~
2.0MPa, reaction time：2 it is small when, the leaching of secondary alkali make in primary slag 98.5%~99.5% molybdenum also in the form of sodium molybdate into
Enter liquid phase, the filtrate that two level press filtration generates returns to dissolving step and utilizes.
2nd, ion exchange
(1) adsorb
Sodium molybdate solution through dissolving and being obtained by filtration, by adding water that feed liquid molybdenum concentration (mass concentration of Mo elements) is dilute
It releases to 10~40g/l, solution is with 5~30m after dilution3The flow of/h is by a kind of anion exchange resin, and molybdenum is with more molybdates
Form be adsorbed onto on resin；Using the resin of clear water washing adsorption saturation, the more molybdates adsorbed on resin also on resin,
It washes away simultaneously remaining containing molybdenum solution in ion exchange column, impurity interference is just avoided that when parsing in next step；Wash water returns thick
Sodium molybdate dilution step；
(2) parse
With saturated ammonium chloride solution (NH4Cl) as parsing agent, with 2.5~15m3The flow velocity of/h to adsorption saturation it is cloudy from
Sub-exchange resin is eluted, parsed, and the more molybdates adsorbed on resin return to solution, is formed ammonium molybdate with ammonia, is obtained
The pure ammonium molybdate solution of 120~180g/l of molybdenum concentration；Clear water washs resin, since the molybdate on resin is replaced
Afterwards, saturated ammonium chloride solution is also remained in ion exchange column, this moieties is come out, the absorption for carrying out a new round is made
Industry.
3rd, crystallize and dry
Pure ammonium molybdate solution obtains ammonium dimolybdate by crystallization, through vacuum filter, using being packaged to be after microwave drying
High-purity ammonium dimolybdate finished product；
The ammonia generated with the absorption by Hydrochloric Acid crystallization process of Wt30%, is made ammonium chloride solution, returns to ion-exchange process
For parsing, recycled so as to fulfill ammonia nitrogen, ammonia nitrogen zero-emission.
Fig. 2 produces ammonium molybdate process flow chart for ion-exchange of the present invention.
The brief mechanism of ion-exchange production ammonium molybdate of the present invention：With highly basic (such as caustic soda NaOH) when raw material containing molybdenum leaches
It decomposes, pickling impurity removal, ammonia leaching instead of classical approach complexity etc., thus leaches obtained thick sodium molybdate solution and do not contain ammonia nitrogen；
Thick sodium molybdate solution is handled by dilution, by the absorption of anion exchange resin, is washed, take full advantage of resin to difference from
The different characteristic of sub- affinity effectively removes foreign ion W, Cu, Ca, S, P, As, Si etc., selects parsing agent NH4Cl solution into
Row parsing, realizes the transition of molybdenum, the substance before absorption is sodium molybdate, is obtained after parsing as pure ammonium molybdate solution；Pure molybdic acid
Ammonium salt solution crystallizes under condition of negative pressure, and the ammonia of generation uses Wt:30% hydrochloric acid is absorbed, and it is molten that saturated ammonium chloride is made
Liquid returns to ion-exchange process and is used as parsing agent.
The foregoing is merely the preferred embodiments of the present invention, are not intended to limit the invention, in the spiritual and former of invention
Any modifications, equivalent replacements and improvements are made within then should be included within the system structure and method of the present invention.
Claims (2)
1. the technique that a kind of ion-exchange produces high-purity ammonium dimolybdate, which is characterized in that comprise the following steps：First, sodium molybdate
It is prepared by solution：(1) dissolving, (two) filtering and secondary leaching；2nd, ion exchange：(1) absorption, (two) parsing；3rd, crystallization and
Drying.
2. the technique that ion-exchange according to claim 1 produces high-purity ammonium dimolybdate, which is characterized in that specific steps
It is as follows：
First, prepared by sodium molybdate solution
(1) dissolve：
By molybdenum raw material in dissolving tank with NaOH solution with molybdenum alkali molar ratio 1:1~1:2 ratio mixing, in temperature 70~100
DEG C, solid-to-liquid ratio 1:5~1：When reaction 2~3 is small under conditions of 10, thick sodium molybdate slurry is made, a part of solvable molybdenum and caustic soda are anti-
Sodium molybdate should be generated and be stored in solution, the undissolved molybdate compound of another part then stays in slag phase；
The molybdenum raw material is industrial molybdenum trioxide, molybdenum dioxide, molybdenum sulfide, molybdate any of which or arbitrary a variety of mixed
Close material；
(2) filtering and secondary leaching：
Thick sodium molybdate slurry is obtained after dissolving to filter by filter press, obtains clear liquid and primary slag；Clear liquid is thick sodium molybdate solution；
In the primary slag of different material containing molybdenum between 5%~20%；The primary slag of leaching is according to solid-to-liquid ratio 1:3~1:5th, basicity 50~
200g/l carries out slurrying, is soaked using secondary alkali, and reaction condition is：200~220 DEG C, 1.5~2.0MPa of partial pressure of oxygen of temperature, instead
Between seasonable：2 it is small when, the leaching of secondary alkali makes in primary slag 98.5%~99.5% molybdenum also enter liquid phase in the form of sodium molybdate, two
The filtrate that grade press filtration generates returns to dissolving step and utilizes；
2nd, ion exchange
(1) adsorb
Sodium molybdate solution through dissolving and being obtained by filtration, by adding water that feed liquid Mo elemental mass concentrations are diluted to 10~40g/l,
Solution is with 5~30m after dilution3The flow of/h is adsorbed onto tree by a kind of anion exchange resin, molybdenum in the form of more molybdates
On fat；Using the resin of clear water washing adsorption saturation, the more molybdates adsorbed on resin wash away ion friendship also on resin
It changes remaining containing molybdenum solution in column；Wash water returns to thick sodium molybdate dilution step；
(2) parse
Using saturated ammonium chloride solution as parsing agent, with 2.5~15m3The flow velocity of/h to the anion exchange resin of adsorption saturation into
Row elution, parsing, the more molybdates adsorbed on resin return to solution, and ammonia formation ammonium molybdate, obtain molybdenum concentration 120~
The pure ammonium molybdate solution of 180g/l；Resin is washed with clear water, washes away remaining saturated ammonium chloride solution, to carry out next round
Adsorption operation；
3rd, crystallize and dry
Pure ammonium molybdate solution obtains ammonium dimolybdate by crystallization, high-purity using being packaged to be after microwave drying through vacuum filter
Ammonium dimolybdate finished product；The ammonia generated with the absorption by Hydrochloric Acid crystallization process of Wt30%, is made ammonium chloride solution, returns to ion exchange
Process recycles, ammonia nitrogen zero-emission for parsing so as to fulfill ammonia nitrogen.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108622938A (en) * | 2018-07-23 | 2018-10-09 | 安徽华西稀有金属材料有限公司 | A method of preparing ammonium dimolybdate from containing molybdenum solution |
| CN109179506A (en) * | 2018-09-21 | 2019-01-11 | 中国地质科学院郑州矿产综合利用研究所 | Method for synergistically recovering rhenium and molybdenum from molybdenum concentrate roasting leacheate |
| CN109650447A (en) * | 2019-01-31 | 2019-04-19 | 成都虹波钼业有限责任公司 | A kind of production of molybdic ammonium technique of environment-friendly high-efficiency |
| CN109775760A (en) * | 2019-03-11 | 2019-05-21 | 中国有色金属工业西安勘察设计研究院有限公司 | Ultralow potassium ammonium molybdate solution, ammonium molybdate solution derived product and preparation method thereof |
| CN110127761A (en) * | 2019-06-24 | 2019-08-16 | 安庆市月铜钼业有限公司 | A kind of ammonium molybdate method for crystallising |
| CN110950384A (en) * | 2019-12-23 | 2020-04-03 | 成都鼎泰新材料有限责任公司 | Method for preparing ammonium molybdate by calcium molybdate raw material ammonium bicarbonate mixed liquid transformation method |
| CN111014713A (en) * | 2019-12-10 | 2020-04-17 | 金堆城钼业股份有限公司 | Preparation method of molybdenum powder |
| CN112174209A (en) * | 2020-09-17 | 2021-01-05 | 成都鼎泰新材料有限责任公司 | Green molybdenum smelting ion exchange process |
| CN112850790A (en) * | 2021-02-01 | 2021-05-28 | 成都虹波钼业有限责任公司 | Molybdenum trioxide for high-solubility catalyst and production process thereof |
| CN114275817A (en) * | 2021-12-16 | 2022-04-05 | 金堆城钼业股份有限公司 | Method for reducing sodium and chlorine content in ammonium dimolybdate |
| CN114275816A (en) * | 2021-12-15 | 2022-04-05 | 成都虹波钼业有限责任公司 | Molybdic acid and production process thereof |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108622938A (en) * | 2018-07-23 | 2018-10-09 | 安徽华西稀有金属材料有限公司 | A method of preparing ammonium dimolybdate from containing molybdenum solution |
| CN109179506A (en) * | 2018-09-21 | 2019-01-11 | 中国地质科学院郑州矿产综合利用研究所 | Method for synergistically recovering rhenium and molybdenum from molybdenum concentrate roasting leacheate |
| CN109650447A (en) * | 2019-01-31 | 2019-04-19 | 成都虹波钼业有限责任公司 | A kind of production of molybdic ammonium technique of environment-friendly high-efficiency |
| CN109775760B (en) * | 2019-03-11 | 2021-10-01 | 中国有色金属工业西安勘察设计研究院有限公司 | Ultra-low potassium ammonium molybdate solution, ammonium molybdate solution derivative product and preparation method thereof |
| CN109775760A (en) * | 2019-03-11 | 2019-05-21 | 中国有色金属工业西安勘察设计研究院有限公司 | Ultralow potassium ammonium molybdate solution, ammonium molybdate solution derived product and preparation method thereof |
| CN110127761A (en) * | 2019-06-24 | 2019-08-16 | 安庆市月铜钼业有限公司 | A kind of ammonium molybdate method for crystallising |
| CN111014713A (en) * | 2019-12-10 | 2020-04-17 | 金堆城钼业股份有限公司 | Preparation method of molybdenum powder |
| CN110950384A (en) * | 2019-12-23 | 2020-04-03 | 成都鼎泰新材料有限责任公司 | Method for preparing ammonium molybdate by calcium molybdate raw material ammonium bicarbonate mixed liquid transformation method |
| CN112174209A (en) * | 2020-09-17 | 2021-01-05 | 成都鼎泰新材料有限责任公司 | Green molybdenum smelting ion exchange process |
| CN112174209B (en) * | 2020-09-17 | 2022-09-30 | 成都虹波钼业有限责任公司 | Green molybdenum smelting ion exchange process |
| CN112850790A (en) * | 2021-02-01 | 2021-05-28 | 成都虹波钼业有限责任公司 | Molybdenum trioxide for high-solubility catalyst and production process thereof |
| CN114275816A (en) * | 2021-12-15 | 2022-04-05 | 成都虹波钼业有限责任公司 | Molybdic acid and production process thereof |
| CN114275817A (en) * | 2021-12-16 | 2022-04-05 | 金堆城钼业股份有限公司 | Method for reducing sodium and chlorine content in ammonium dimolybdate |
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Application publication date: 20180529 |