CN1123335A - Lead-removing method for ammonium salt refined by antimony affination process - Google Patents
Lead-removing method for ammonium salt refined by antimony affination process Download PDFInfo
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- CN1123335A CN1123335A CN 94113150 CN94113150A CN1123335A CN 1123335 A CN1123335 A CN 1123335A CN 94113150 CN94113150 CN 94113150 CN 94113150 A CN94113150 A CN 94113150A CN 1123335 A CN1123335 A CN 1123335A
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- ammonium salt
- antimony
- deleading
- ammonia
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Abstract
The present invention relates to an deleading method for ammonium salt by antimony pyrorefining. Its production process is as follows: it uses phosphoric oxyacid ammonium salt and sulfuric oxyacid ammonium salt or compounded ammonium salt of the above-mentioned both ammonium salts as deleading agent. its temp. is controlled between 700-1100 deg.C, and the constant temp. is kept for above half a hour, and then such procedures of removing surface dross, sampling analysis and cooling are carried out, so that the refined antimony can be obtained.
Description
The present invention relates to a kind of method for removing lead that needle antimony is carried out pyrorefining.
In the pyrorefining antimony process, its associated metallic lead major part enters in the needle antimony, and the finished product star metal or stibium trioxide have certain requirement to the content of lead, and star metal requires lead tolerance 0.1～0.2%, and stibium trioxide requires lead tolerance less than 0.1%.To reach such standard undoubtedly, must carry out the refining lead-removing operation needle antimony.At present, the method for removing lead of pertinent data introduction has vacuum distillation method, chlorination process and liquation process.The vacuum distillation method deleading is effective, but the equipment complexity; The chlorination process direct yield is low, and environmental pollution is serious; Liquation process throughput is little, only the production of suitable high purity antimony.Therefore, still there are not a kind of economical rationality, effective method for removing lead so far.
Application number is in " stibium fire refining deleading agent and preparation thereof and application " patent application of 94111122.9, boron, phosphorus, the silicon oxysalt displacement deleading method of antimony have been adopted, exist deleading agent complex manufacturing, production cost height, the deleading effect is not good enough, weak points such as the slag rate is big, and direct yield is low.
The purpose of this invention is to provide a kind of ammonium salt deleading method that is used for fire refining of antimony, accomplish that deleading agent prepares easily, application apparatus is simple, deleading is effective, the direct yield height.
The present invention adopts phosphorus oxyacid ammonium salt, sulphur oxygen acid ammonium salt or the ammonium salt compound of the two as deleading agent.Compound ammonia salt during as deleading agent its weight proportion be phosphorus oxyacid ammonium salt 40%～70%, sulphur oxygen acid ammonium salt 30～60%.The deleading principle is to utilize ammonium salt or ammonium salt compound at high temperature unstable, easily decomposes and emits ammonia.Like this, remaining on the one hand acid anhydrides and the lead in the needle antimony are combined to corresponding salt and enter scum silica frost, reach plumbous, antimony separation; The ammonia of emitting on the other hand fully stirs the antimony liquation, quickens the carrying out of chemical reaction.Processing step of the present invention and deleading process are as follows:
One, electric furnace deleading method
In the antimony regulus of fragmentation is packed crucible at first a little, ammonium salt or ammonium salt compound are covered from the teeth outwards as the deleading agent slag, heat up then.More than temperature reaches the ammonium salt fusing point, when antimon point is following, ammonium salt fusing and antimony does not melt, the ammonium salt liquation arrives crucible bottom by the slit of antimony regulus.Along with the rising of temperature, antimony regulus begins fusing.Since the proportion of antimony liquation greater than ammonium salt solution proportion, therefore form the antimony liquation downwards, the countercurrent flow that makes progress of ammonium salt liquation with contact.When temperature was raised to temperature between 700～1100 ℃, constant temperature was more than half an hour, removed out surface scum again, the temperature cooling is removed in the qualified back of sampling analysis, obtains star metal.
Ammonia salt or ammonium salt compound add-on are decided according to the percentage composition of lead, if the final lead tolerance of star metal is controlled at below 0.15%, add-on is calculated by following formula:
g＝100k.X
G is the deleading agent weight that antimony per ton should add in the formula, the unit kilogram
X is the lead tolerance of needle antimony
K is a constant, is generally 10～35, can decide as the case may be.
Two, reverberatory furnace deleading method
After the antimony regulus reverberatory furnace contains the fusing of plumbic antimony, ammonia salt or compound ammonia salt are covered at the antimony molten surface as deleading agent, be warmed up on the temperature between 700～1100 ℃, and air blast is stirred the antimony liquation more than half an hour, claw surface scum, put the antimony mold after sampling analysis is qualified.
As the ammonium salt compound of deleading agent can be on the market phosphorus oxyacid ammonia salt and sulphur oxygen acid ammonia salt are mixed by a certain percentage and to get, but capable the best that is prepared as of order chemically.
It is as follows that compound ammonia salinization length of schooling is equipped with step: earlier sulphur, phosphorus oxyacid are mixed according to a certain ratio, carry out neutralization reaction with ammonia or bicarbonate of ammonia, again through concentrate, crystallization, drying process and make.
Compared with the prior art the present invention has following characteristics:
1, as the ammonia salt or the compound ammonia salt wide material sources of deleading agent, preparation promptly can prepare with chemical process easily voluntarily.
2, can directly utilize original fire refining of antimony facility, not increase new equipment basically, promptly application apparatus is simple, economically feasible.
3, direct yield height, deleading is effective, not only can remove lead, can also remove impurity such as iron, copper, zinc, aluminium.
Embodiment one: the antimony regulus of 100 grams leaded 2.53% is put into crucible, compound ammonia salt 8 grams that adding is made up of 60% phosphorus oxyacid ammonium salt, 40% sulphur oxygen acid ammonium salt, crucible sent into be warmed up to 700 ℃ in the muffle furnace, constant temperature half an hour, the cooling cooling can obtain lead tolerance less than 0.09% star metal.
Embodiment two: the antimony regulus of 5000 grams leaded 2.53% is put into the silicon carbide crucible that is wound with resistance wire, add compound ammonia salt 400 grams of being made up of 40% phosphorus oxyacid ammonium salt, 60% sulphur oxygen acid ammonium salt, energising is warming up to 900 ℃.Constant temperature 1 hour claws surface scum, sampling analysis, and cooling cooling can obtain lead tolerance less than 0.13% star metal.
Embodiment three adds 36 tons of leaded 1.46% antimony regulus in industrial reverberatory furnace, add 1.1 tons of the compound ammonia salt formed by 70% phosphorus oxyacid ammonium salt, 30% sulphur oxygen acid ammonium salt after the heat fused again, temperature is controlled at 850 ℃, air blast 2 hours, claw surface scum, sampling analysis can obtain lead tolerance less than 0.16% star metal after the cooling.
Embodiment four
Basically identical with example three, just the deleading agent that adds is made up of 70% phosphorus oxyacid ammonium salt, 25% sulphur oxygen acid ammonium salt, 5% chlorine oxygen acid ammonium salt.
Embodiment five
Basically identical with example three, just temperature is controlled at 1100 ℃.
Embodiment six
Basically identical with example one, just deleading agent is used phosphorus oxyacid ammonia salt separately.The deleading effect is a little less than example one.
Embodiment seven
Basically identical with example one, just deleading agent is used sulphur oxygen acid ammonia salt separately, and the deleading effect is lower than above-mentioned whole embodiment.
Claims (3)
1, a kind of ammonia salt deleading method that is used for fire refining of antimony, it is characterized in that using the phosphorus oxyacid ammonium salt, sulphur oxygen acid ammonium salt or the ammonium salt compound of the two are as deleading agent, temperature is controlled on the temperature between 700～1100 ℃, constant temperature is more than half an hour, remove out surface scum, sampling analysis, cooling cooling and obtain star metal.
2, method according to claim 1 is characterized in that compound ammonia salt mainly is made up of two kinds of oxygen acid ammonium salts of p and s, and weight proportion is a phosphorous oxyacid hydrochlorate 40～70%, sulphur oxygen acid ammonium salt 30～60%.
3, method according to claim 1 and 2, its feature in the best preparation process of ammonium salt compound is: earlier the sulphur phosphorus oxyacid is mixed according to a certain ratio, carries out neutralization reaction with ammonia or bicarbonate of ammonia, again through concentrate, crystallization, drying process and make.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94113150 CN1123335A (en) | 1994-11-25 | 1994-11-25 | Lead-removing method for ammonium salt refined by antimony affination process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94113150 CN1123335A (en) | 1994-11-25 | 1994-11-25 | Lead-removing method for ammonium salt refined by antimony affination process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1123335A true CN1123335A (en) | 1996-05-29 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 94113150 Pending CN1123335A (en) | 1994-11-25 | 1994-11-25 | Lead-removing method for ammonium salt refined by antimony affination process |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1047407C (en) * | 1995-01-25 | 1999-12-15 | 刘伯龙 | High-efficiency deleading method and liquid deleading agent for fire refining of antimony |
| CN101265520B (en) * | 2008-05-06 | 2010-06-09 | 锡矿山闪星锑业有限责任公司 | Treatment method for refining lead slag-removed by antimony fire refining process |
| CN102041399A (en) * | 2010-12-06 | 2011-05-04 | 益阳市华昌锑业有限公司 | Antimony fire refining lead-removal agent and application thereof |
| CN102560150A (en) * | 2012-02-13 | 2012-07-11 | 锡矿山闪星锑业有限责任公司 | Efficient lead removing agent for fire refining antimony and preparation method and application of efficient lead removing agent |
| CN106244836A (en) * | 2016-08-26 | 2016-12-21 | 益阳生力材料科技股份有限公司 | A kind of method for removing cadmium of antimony alloy |
-
1994
- 1994-11-25 CN CN 94113150 patent/CN1123335A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1047407C (en) * | 1995-01-25 | 1999-12-15 | 刘伯龙 | High-efficiency deleading method and liquid deleading agent for fire refining of antimony |
| CN101265520B (en) * | 2008-05-06 | 2010-06-09 | 锡矿山闪星锑业有限责任公司 | Treatment method for refining lead slag-removed by antimony fire refining process |
| CN102041399A (en) * | 2010-12-06 | 2011-05-04 | 益阳市华昌锑业有限公司 | Antimony fire refining lead-removal agent and application thereof |
| CN102560150A (en) * | 2012-02-13 | 2012-07-11 | 锡矿山闪星锑业有限责任公司 | Efficient lead removing agent for fire refining antimony and preparation method and application of efficient lead removing agent |
| CN102560150B (en) * | 2012-02-13 | 2013-09-11 | 锡矿山闪星锑业有限责任公司 | Efficient lead removing agent for fire refining antimony and preparation method and application of efficient lead removing agent |
| CN106244836A (en) * | 2016-08-26 | 2016-12-21 | 益阳生力材料科技股份有限公司 | A kind of method for removing cadmium of antimony alloy |
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