CN103387264B - Comprehensive utilization method of molybdenum in waste molybdenum - Google Patents
Comprehensive utilization method of molybdenum in waste molybdenum Download PDFInfo
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- CN103387264B CN103387264B CN201310323552.1A CN201310323552A CN103387264B CN 103387264 B CN103387264 B CN 103387264B CN 201310323552 A CN201310323552 A CN 201310323552A CN 103387264 B CN103387264 B CN 103387264B
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Abstract
The invention relates to a comprehensive utilization method of molybdenum in waste molybdenum. The comprehensive utilization method comprises the following steps of: (S1) preprocessing the waste molybdenum; (S2) adjusting concentration of molybdenum acid pickle; (S3) adding the molybdenum acid pickle of which the concentration is adjusted into molybdenum mud, stirring for reacting in an enamel reaction vessel for 2 hours under the conditions that the initial temperature is 40-50 DEG C, the pressure is normal pressure and the stirring speed is 110 revolution/minute; (S4) regulating the pH to 1 by utilizing ammonium hydroxide so as to prepare molybdic acid; and (S5) filtering and separating the molybdic acid by utilizing a centrifugal machine or a compressor. By recycling and producing molybdenum products by utilizing the comprehensive utilization method, high economic benefit and remarkable social benefit are obtained.
Description
Technical field
The present invention relates in useless molybdenum (molybdenum acid pickle and molybdenum mud) molybdenum method of comprehensive utilization.
Background technology
At present, the relevant electric light source industry of China, such as produces the enterprise of energy-saving filament, in the production process of its energy-saving filament
In, have substantial amounts of waste liquid containing molybdenum to produce, its waste liquid amount containing molybdenum at 40-80 g/l, nitric acid content 3-5mol/L, acidity is relatively
By force.Process to this liquid, early discarded before this, with the method for ammonia neutralization, useless molybdenum was made molybdic acid more later, and then is reprocessed into molybdenum
The molybdenum products such as sour ammonium, sodium molybdate are used.In ammonia, legal shortcoming is that ammonia consumption is big, produces one ton of ammonium molybdate product and uses
More than two tons of ammonia, high processing costs (producing one ton of ammonium molybdate needs ammonia cost to want more than 10,000 yuan).
The relevant molybdenum product deep processing industry of China, the such as manufacturing enterprise such as Mo wafer, during processing Mo wafer,
Produce a certain amount of waste material containing molybdenum, be commonly called as " molybdenum mud " or " emery wheel ash ".Its amount containing molybdenum is between 40%-60%.To this molybdenum
The regeneration of waste material, domestic at present method used be waste material is pulverized after, become oxygen with raw coal roasting oxidation in roaster
Change molybdenum, be reprocessed into the molybdenum products such as ammonium molybdate.The shortcoming of this law is that matchmaker's roasting oxidation process is slow, coal consumption big, and discharges a large amount of
Carbon dioxide.Production cost is high, and molybdenum loss is big, is unfavorable for reducing discharging and environmental protection.
Content of the invention
Technical problem solved by the invention is to provide the method for comprehensive utilization of molybdenum in useless molybdenum, thus solving above-mentioned background
Problem in technology.
Technical problem solved by the invention employs the following technical solutions to realize：
In useless molybdenum, the method for comprehensive utilization of molybdenum, comprises the steps：
S1, useless molybdenum is pre-processed：Molybdenum mud is carried out just aoxidize and pulverize, the polishing in molybdenum circle is the state in water mill
Under carry out, after the water decantation received in mud bucket, molybdenum mud is met air and is just gradually oxidized to molybdenum dioxide, is dried afterwards again,
Be ground into granularity in 15-20 mesh, should not be too thin, no reaction too strong it is difficult to control；
S2, concentration adjustment is carried out to molybdenum acid pickle, refer to that in molybdenum acid pickle, concentration of nitric acid measures and adjustment, with added
The weight of molybdenum mud calculates, the weight 10%-20% many compared with the weight of molybdenum mud of nitric acid, and nitric acid refers to the nitric acid that concentration is 3mol/L；
S3, add the molybdenum acid pickle after concentration adjustment in molybdenum mud, and put in enamel reaction pot and reacted, initial
Temperature 40-50 DEG C, normal pressure, stirs under 110 revs/min, 2 hours reaction time；
S4, with ammoniacal liquor adjust pH=1 molybdic acid；
S5, use centrifuge or compressor filtration separation molybdic acid.
Then according to molybdic acid is processed ammonium molybdate and sodium molybdate by the technique of routine, spent ion exchange resin extracts tail washings simultaneously
In a small amount of molybdenum.
According to the problem existing in terms of the domestic at present recycling in waste liquid containing molybdic acid and molybdenum mud (emery wheel ash), that is, produce
High cost, environmental pollution is big, the problems such as molybdenum loss is many.Find out the chemical characteristic of two useless (useless molybdic acid liquid, useless molybdenum mud) by experiment
Difference, that is, the molybdenum liquid that gives up has an oxidisability (containing nitric acid) and molybdenum mud has reproducibility (main component of molybdenum mud is molybdenum dioxide
MoO2), create certain condition, make them organically carry out chemical reaction, thus reaching the purpose decomposed using reclaiming molybdenum.Useless
Molybdenum decomposes makes molybdic acid, further makes the molybdenum products such as ammonium molybdate, sodium molybdate.Useless molybdenum is made to move towards regeneration, recycle
Way, reaches the purpose of " method two molybdenum ".This law has the advantages that to react fast, low cost, molybdenum high income and environmental pollution is little.
Chemical reaction and reaction equation：
MoO2+2HNO3=H2MoO4+2NO2
Compared with the recoverying and utilizing method of former waste liquid containing molybdic acid and molybdenum mud, the significant advantage of the art of this patent is：
1st, the molybdenum that gives up reclaims processing cost and significantly reduces, and liquefied ammonia consumption reduces 75%-80%, without roasting without coal, ton molybdenum
Product (ammonium molybdate) processing cost saves more than ten thousand yuan.
2nd, chemical time is short, and process time is short, improves production efficiency.
3rd, Whote-wet method puies forward molybdenum, molybdenum high income, and molybdenum yield is more than 98%.
4th, non-carbon-emitting, environmental protection.
In recent years, applicant place factory obtains preferably economic effect using the art of this patent remanufacture molybdenum product
Benefit, also achieves significant social benefit simultaneously.
Brief description
Fig. 1 is flow chart of the present invention.
Specific embodiment
In order that technological means, creation characteristic, reached purpose and effect that the present invention realizes are easy to understand, tie below
Conjunction is specifically illustrating, and the present invention is expanded on further.
Embodiment 1
Referring to Fig. 1, in useless molybdenum, the method for comprehensive utilization of molybdenum, comprises the steps：
S1, useless molybdenum is pre-processed：Molybdenum mud is carried out just aoxidize and pulverize, the polishing in molybdenum circle is the state in water mill
Under carry out, after the water decantation received in mud bucket, molybdenum mud is met air and is just gradually oxidized to molybdenum dioxide, is dried afterwards again,
Be ground into granularity in 20 mesh, should not be too thin, no reaction too strong it is difficult to control.
S2, concentration adjustment is carried out to molybdenum acid pickle, refer to that in molybdenum acid pickle, concentration of nitric acid measures and adjustment, with added
The weight of molybdenum mud calculates, the weight 10%-20% many compared with the weight of molybdenum mud of nitric acid, and nitric acid refers to the nitric acid that concentration is 3mol/L；
S3, add the molybdenum acid pickle after concentration adjustment in molybdenum mud, and put in enamel reaction pot and reacted, initial
Temperature 50 C, normal pressure, stirs under 110 revs/min, 2 hours reaction time；
S4, with ammoniacal liquor adjust pH=1 molybdic acid；
S5, use centrifuge or compressor filtration separation molybdic acid.
Then according to molybdic acid is processed ammonium molybdate and sodium molybdate by the technique of routine, spent ion exchange resin extracts tail washings simultaneously
In a small amount of molybdenum.
Embodiment 2
In a kind of useless molybdenum, the method for comprehensive utilization of molybdenum, comprises the steps：
S1, useless molybdenum is pre-processed：Molybdenum mud is carried out just aoxidize and pulverize, the polishing in molybdenum circle is the state in water mill
Under carry out, after the water decantation received in mud bucket, molybdenum mud is met air and is just gradually oxidized to molybdenum dioxide, is dried afterwards again,
Be ground into granularity in 15 mesh, should not be too thin, no reaction too strong it is difficult to control.
S2, concentration adjustment is carried out to molybdenum acid pickle, refer to that in molybdenum acid pickle, concentration of nitric acid measures and adjustment, with added
The weight of molybdenum mud calculates, and 10% more than the weight of molybdenum mud, nitric acid refers to the nitric acid that concentration is 3mol/L to the weight of nitric acid；
S3, add the molybdenum acid pickle after concentration adjustment in molybdenum mud, and put in enamel reaction pot and reacted, initial
Temperature 50 C, normal pressure, stirs under 110 revs/min, 2 hours reaction time；
S4, with ammoniacal liquor adjust pH=1 molybdic acid；
S5, use centrifuge or compressor filtration separation molybdic acid.
Then according to molybdic acid is processed ammonium molybdate and sodium molybdate by the technique of routine, spent ion exchange resin extracts tail washings simultaneously
In a small amount of molybdenum.
Embodiment 3
In a kind of useless molybdenum, the method for comprehensive utilization of molybdenum, comprises the steps：
S1, useless molybdenum is pre-processed：Molybdenum mud is carried out just aoxidize and pulverize, the polishing in molybdenum circle is the state in water mill
Under carry out, after the water decantation received in mud bucket, molybdenum mud is met air and is just gradually oxidized to molybdenum dioxide, is dried afterwards again,
Be ground into granularity in 17 mesh, should not be too thin, no reaction too strong it is difficult to control.
S2, concentration adjustment is carried out to molybdenum acid pickle, refer to that in molybdenum acid pickle, concentration of nitric acid measures and adjustment, with added
The weight of molybdenum mud calculates, and 15% more than the weight of molybdenum mud, nitric acid refers to the nitric acid that concentration is 3mol/L to the weight of nitric acid；
S3, add the molybdenum acid pickle after concentration adjustment in molybdenum mud, and put in enamel reaction pot and reacted, initial
Temperature 50 C, normal pressure, stirs under 110 revs/min, 2 hours reaction time；
S4, with ammoniacal liquor adjust pH=1 molybdic acid；
S5, use centrifuge or compressor filtration separation molybdic acid.
Then according to molybdic acid is processed ammonium molybdate and sodium molybdate by the technique of routine, spent ion exchange resin extracts tail washings simultaneously
In a small amount of molybdenum.
General principle and principal character and the advantages of the present invention of the present invention have been shown and described above.The technology of the industry
, it should be appreciated that the present invention is not restricted to the described embodiments, the simply explanation described in above-described embodiment and specification is originally for personnel
The principle of invention, without departing from the spirit and scope of the present invention, the present invention also has various changes and modifications, these changes
Change and improvement both falls within scope of the claimed invention.Claimed scope by appending claims and its
Equivalent thereof.
Claims (1)
1. give up molybdenum in molybdenum method of comprehensive utilization it is characterised in that：Comprise the steps：
S1, useless molybdenum carried out just aoxidize and pulverize, wherein useless molybdenum is molybdenum mud：Polishing in molybdenum circle is to carry out in the state of water mill
, after the water decantation received in mud bucket, molybdenum mud is met air and is just gradually oxidized to molybdenum dioxide, is dried afterwards again, is ground into
Granularity is in 15-20 mesh；
S2, concentration adjustment is carried out to molybdenum acid pickle, refer to the mensure of concentration of nitric acid and adjustment in molybdenum acid pickle, with the molybdenum being added
Mud weight calculates, the weight 10%-20% many compared with the weight of molybdenum mud of nitric acid, and nitric acid refers to the nitric acid that concentration is 3mol/L；
S3, to S1In first oxidation and pulverize after molybdenum mud in, add concentration adjustment after molybdenum acid pickle, and put into enamel reaction
Reacted in pot, in 40 DEG C -50 DEG C of initial temperature, normal pressure, stirred under 110 revs/min, 2 hours reaction time；
S4, with ammoniacal liquor adjust pH=1 molybdic acid；
S5, use centrifuge or Filter Press separation molybdic acid.
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| CN104141047B (en) * | 2013-09-27 | 2016-05-11 | 开封新巨源环保科技开发有限公司 | A kind of recycling processing method of molybdenum iron slag |
| CN108017089B (en) * | 2017-12-11 | 2019-08-02 | 宁夏共宣环保科技有限责任公司 | A method of recycling ammonium molybdate from useless molybdenum catalyst |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RO122632B1 (en) * | 2005-06-07 | 2009-10-30 | Institutul De Cercetări În Chimie "Raluca Ripan" | Process for obtaining molybdenic acid from molybdenum wastes |
| CN101760652A (en) * | 2009-12-29 | 2010-06-30 | 广东省矿产应用研究所 | Technological method for treating refractory complex molybdenum ore by combined dressing and smelting process |
| CN101780978A (en) * | 2009-01-15 | 2010-07-21 | 自贡硬质合金有限责任公司 | Method for recycling sodium molybdate solution from molybdenum contained silica slag |
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| JPH0236533B2 (en) * | 1986-03-24 | 1990-08-17 | Kogyo Gijutsuin | MORIBUDENSANENGANJUSUIYOEKIKARAMORIBUDENSANENOKAISHUSURUHOHO |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RO122632B1 (en) * | 2005-06-07 | 2009-10-30 | Institutul De Cercetări În Chimie "Raluca Ripan" | Process for obtaining molybdenic acid from molybdenum wastes |
| CN101780978A (en) * | 2009-01-15 | 2010-07-21 | 自贡硬质合金有限责任公司 | Method for recycling sodium molybdate solution from molybdenum contained silica slag |
| CN101760652A (en) * | 2009-12-29 | 2010-06-30 | 广东省矿产应用研究所 | Technological method for treating refractory complex molybdenum ore by combined dressing and smelting process |
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