CN103866121A - Method for preparing sodium antimonate from antimony oxide ore via alkaline approach - Google Patents
Method for preparing sodium antimonate from antimony oxide ore via alkaline approach Download PDFInfo
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- CN103866121A CN103866121A CN201410107329.8A CN201410107329A CN103866121A CN 103866121 A CN103866121 A CN 103866121A CN 201410107329 A CN201410107329 A CN 201410107329A CN 103866121 A CN103866121 A CN 103866121A
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Abstract
The invention discloses a method for preparing sodium antimonate from an antimony oxide ore via an alkaline approach. The method comprises the following steps: (1) leaching the antimony oxide ore, (2) purifying filtrate, and (3) oxidizing the purified filtrate. The method is high in recovery rate, the leaching rate of antimony is 95-99%, the direct recovery rate of sodium antimonate is 90-95%, the whole process is performed under an alkaline environment, the requirement on corrosion resistance of equipment is not high, no complicated pretreatment is required in the process, the needed raw materials are nontoxic and harmless, the alkaline liquid is recyclable, neither waste water nor waste gas is generated in the process, and waste residues are nontoxic and harmless.
Description
Technical field
The present invention relates to a kind of method of preparing sodium antimonate, especially relate to a kind of method that antimony oxide ore alkaline process is prepared sodium antimonate.
Background technology
Antimony oxide ore is a kind of unmanageable ore deposit, and when low-grade antimony oxide ore carries out ore dressing, its rate of recovery is low, and when, the antimony grade in raw ore is below 10%, while obtaining 30% grade by ore dressing, its rate of recovery is 50% left and right; It is 30% when above that the antimony oxide ore of 10-20% is brought up to grade by ore dressing, and its rate of recovery is 60% left and right; Therefore, generally process the antimony oxide ore of 10-20%, often adopt pyrogenic process to carry out.If the antimony oxide ore of 10-20% grade is directly carried out to straight well stove pyrometallurgical smelting, the evaporation rate of antimony is 50-60%; If antimony oxide ore fine grinding, below 2mm, is mixed and made into cellular artificial type lump ore with coal, dry after, then in straight well stove in the 900-1050 DEG C of smelting of volatilizing, its rate of recovery is 70-80%, in this method process, the rate of recovery of antimony is not high yet.
Summary of the invention
The technical problem to be solved in the present invention is, overcomes in prior art and processes the not high deficiency of the rate of recovery that grade exists in the time of the antimony oxide ore of 10-20%, provides that a kind of rate of recovery is higher, the antimony oxide ore alkaline process of less pollution is prepared the method for sodium antimonate.
The technical scheme that the present invention solves its technical problem employing is that a kind of antimony oxide ore alkaline process is prepared the method for sodium antimonate, specifically comprises the following steps:
(1) antimony oxide ore leaches: antimony oxide ore is crushed to-150 orders, then leaches with sodium hydroxide solution, add suitable reductive agent, maintenance temperature is 80-100 DEG C, and extraction time is 60-120 minute; Then filter, obtain filter residue and filtrate, filtrate is the sodium hydroxide solution containing antimony;
Antimony content in gained filter residue is very low, stores up or for manufacture of cement materials as waste residue, and filtrate purifies for next procedure;
The composition of described antimony oxide ore is: antimony 10-20wt%, iron 10-20wt%, plumbous 1-3wt%, arsenic 0.1-0.5wt%;
(2) filtrate purifies: in step (1) gained filtrate, add scavenging agent, the add-on of described scavenging agent is the 18-40% that is equivalent to antimony element mass content in feed oxygen antimony sulfide ore, and reaction 30-60 minute, filters, and filtrate is scavenging solution; (add scavenging agent to make the impurity element in leach liquor become precipitation, filter rear and solution separating)
Described scavenging agent is water-soluble mantoquita, preferably sulfuric acid copper or cupric chloride.
The object that adds scavenging agent is the sulfocompound purifying in leach liquor, and the existence of sulfocompound affects the quality of the finished product, is mainly wherein content and the outward appearance that affects principal constituent.Before preparing sodium antimonate, adopt mantoquita to purify to leach liquor, the sulfocompound in leach liquor and cupric ion generate the cupric sulfide that solubility product is very little and separate.
(3) scavenging solution oxidation: add hydrogen peroxide to be oxidized toward step (2) gained scavenging solution at 60-100 DEG C, the add-on of described hydrogen peroxide be equivalent to antimony element quality in scavenging solution 3.0-5.0 doubly, maintenance temperature is 60-100 DEG C, reaction 30-60 minute, filters and obtains wet sodium antimonate and filtrate; By dry wet gained sodium antimonate, obtain product sodium antimonate; Regulate the concentration of sodium hydroxide in filtrate, return to step (1) and leach, recycle.Whole process does not produce waste water.
Further, in step (1), the concentration that leaches sodium hydroxide used is 300-400g/L; The liquid-solid ratio of described sodium hydroxide solution and antimony oxide ore is 10-16ml ︰ 1g; The add-on of reductive agent is decided by tetravalence antimony in antimony oxide ore and antimonic content, the add-on of reductive agent is for to be reduced to antimonious amount by tetravalence antimony and quinquevalence antimony in weisspiessglanz, and the add-on of general reductive agent is equivalent to the 14-30% of antimony oxide ore antimony element quality; Reductive agent generally uses hydrazine hydrate or hydrazonium sulfate, and wherein, hydrazine hydrate is more suitable.
Further, in step (3), the preferred 27.5-60wt% of concentration of described hydrogen peroxide.
The present invention adopts wet method alkali to soak, and directly generates sodium antimonate; Its principle is that the antimonous oxide based in antimony oxide ore is dissolved in hot sodium hydroxide solution, and other impurity is as few in lead, copper, iron etc. dissolve.
Its main chemical reactions is:
In leaching process, need to add a certain amount of reductive agent, impel the high price sb oxide in antimony oxide ore to be reduced to antimonous oxide, and be dissolved in hot sodium hydroxide solution, together leach.Its reaction formula is as follows:
The present invention adopts alkaline Leaching antimony oxide ore, then, purifies leach liquor, and oxidation antimony wherein, obtains sodium antimonate, and alkali lye returns to leaching, recycles, and this method is processed the oxidized ore of antimony, and the rate of recovery is high, does not pollute.
The weisspiessglanz in antimony ore is converted into sodium antimonate by the present invention, and the leaching yield of antimony is 95-99%, and the direct yield of sodium antimonate is 90-95%.Although the iron level in antimony oxide ore is very high, as reach 17% left and right,, adopt sodium hydroxide solution to leach, iron-based does not originally enter in solution, thereby is isolated.The sodium antimonate that the present invention obtains is used as the finings of picture tube, opticglass and various high glasses, the fire retardant of textiles, plastics, enamel opacifier, the composition of the opaque filler of manufacture foundry goods use paint and iron sheet, steel plate acid-proof varniss; In chemical analysis for the identification of receiving ion.
The rate of recovery of present method antimony is high, exceeds 30-35% than current pyrogenic processing method.The obtained sodium antimonate quality of the present invention is higher, and outward appearance is greyish white, and main chemical compositions meets YS/T22-2010 standard.
The whole process of the present invention is carried out in alkaline environment, less demanding to equipment anticorrosion, and process does not have complicated pre-treatment, desired raw material is not poisonous and hazardous material, and alkali lye recycles, and process does not produce waste water, also do not have waste gas to produce, waste residue is nontoxic, and environmental pollution is less.
Embodiment
Below in conjunction with embodiment, the invention will be further described, but technology contents of the present invention is not limited to described scope.
Embodiment 1
The present embodiment comprises the following steps:
(1) antimony oxide ore leaches: antimony oxide ore is crushed to-150 orders, get-150 wherein Sb10.15wt%, As0.15wt%, Pb1.02wt%, Fe17.02wt% of object antimony oxide ore 100g(), add in 1.1L sodium hydroxide solution (NaOH concentration is 300.2g/L), add hydrazonium sulfate 1.5g, 82 ± 2 DEG C of extraction temperatures, extraction time 60 minutes; Then filter, obtain filter residue, dry rear wherein Sb0.51%, Fe20.55% of weight 82g(), wherein Sb9.73g/L of filtrate 1.0L();
(2) filtrate purifies: in step (1) gained filtrate, add copper sulfate 2.0g, under room temperature, stir 30 minutes, filter and be purified liquid 1.0L and purification slag; Gained purification slag dry weight 3.0g(Sb0.04%, Cu21.23%);
(3) scavenging solution oxidation: scavenging solution is warmed up to 62 ± 2 DEG C, add hydrogen peroxide (mass concentration is 30wt%) 30mL, oxidization time 30 minutes, filtration obtains wet sodium antimonate, be dried and obtain dry sodium antimonate 19.2g, its outward appearance is shallow white, and main chemical compositions is: Sb48.20%, As0.06%, Fe0.01%, Cu0.01%, Pb0.03%; Filtrate is the alkali lye 1.1L after oxidation, and its content NaOH245.2g/L turns back to step (1) leaching stage, loops leaching.
In the present embodiment, the leaching yield 95.88% of antimony in antimony oxide ore; Leach, purify again to sodium antimonate from antimony oxide ore, the direct yield of its antimony is 91.25%; The rate of recovery of the copper in the mantoquita in scavenging agent is 80%.
Embodiment 2
The present embodiment comprises the following steps:
(1) antimony oxide ore leaches: antimony oxide ore is crushed to-150 orders, get-150 wherein Sb16.45%, As0.25%, Pb2.51%, Fe16.73% of object antimony oxide ore 200g(), add 2.5L sodium hydroxide solution (NaOH content is 383.5g/L) to leach, add hydrazine hydrate 5.9g, 87 ± 2 DEG C of extraction temperatures, extraction time 70 minutes, then filter, obtain filter residue, dry rear wherein Sb0.33%, Fe22.15% of weight 150g(), wherein Sb14.21g/L of filtrate 2.3L();
(2) filtrate purifies: in step (1) gained filtrate, add cupric chloride 8.2g, under room temperature, stir and purify 35 minutes, filter and be purified liquid 2.3L and purification slag, purification slag dry weight 4.9g(Sb0.08%, Cu55.08%);
(3) scavenging solution oxidation: step (2) gained scavenging solution is warmed up to 72 ± 2 DEG C, add hydrogen peroxide (mass concentration is 60wt%) 118mL, oxidization time 35 minutes, filtration obtains wet sodium antimonate, be dried and obtain dry sodium antimonate 64.2g, its outward appearance is shallow white, and main chemical compositions is: Sb47.98%, As0.09%, Fe0.02%, Cu0.01%, Pb0.03%; Alkali lye 2.9L after oxidation, its content NaOH299.0g/L, turns back to step (1) leaching stage, loops leaching.
In the present embodiment, the leaching yield 98.50% of antimony in antimony oxide ore; Leach, purify again to sodium antimonate from antimony oxide ore, the direct yield of its antimony is 93.56%; The rate of recovery of the copper in the mantoquita in scavenging agent is 70%.
Embodiment 3
The present embodiment comprises the following steps:
(1) antimony oxide ore leaches: antimony oxide ore is crushed to-150 orders, get-150 wherein Sb13.59%, As0.35%, Pb2.68%, Fe18.79% of object antimony oxide ore 250g(), add in 3.4L sodium hydroxide solution (NaOH concentration is 358.9g/L), leach, add hydrazine hydrate 6.8g, 95 ± 2 DEG C of extraction temperatures, extraction time 90 minutes, then filters, and obtains filter residue, wherein Sb0.56%, Fe23.85% of weight 195g(after dry), wherein Sb10.65g/L of filtrate 3.1L();
(2) filtrate purifies: in step (1) gained filtrate, add copper sulfate 10.2g, under room temperature, stir lower purification 45 minutes, filter and be purified slag, its dry weight 8.5g(Sb0.06%, Cu35.83%), scavenging solution 3.1L;
(3) scavenging solution oxidation: step (2) gained scavenging solution is warmed up to 82 ± 2 DEG C, add hydrogen peroxide (mass concentration is 27.5wt%) 139mL, oxidization time 45 minutes, filtration obtains wet sodium antimonate, be dried and obtain dry sodium antimonate 66.8g, its outward appearance is canescence, and main chemical compositions is: Sb48.12%, As0.08%, Fe0.05%, Cu0.02%, Pb0.03%; Alkali lye 3.8L after oxidation, its content NaOH284.7g/L, turns back to step (1) leaching stage, loops leaching.
In the present embodiment, the leaching yield 96.79% of antimony in antimony oxide ore; Leach, purify again to sodium antimonate from antimony oxide ore, the direct yield of its antimony is 94.58%; The rate of recovery of the copper in the mantoquita in scavenging agent is 75%.
Embodiment 4
The present embodiment comprises the following steps:
(1) antimony oxide ore leaches: antimony oxide ore is crushed to-150 orders, get-150 wherein Sb17.78%, As0.28%, Pb1.86%, Fe10.45% of object antimony oxide ore 300g(), add in 4.7L sodium hydroxide solution (NaOH concentration is 334.6g/L) and leach, add hydrazine hydrate 13.3g, 82 ± 2 DEG C of extraction temperatures, extraction time 110 minutes, then filter, obtain filter residue, dry rear wherein Sb0.28%, Fe14.37% of weight 216g(), wherein Sb12.34g/L of filtrate 4.3L();
(2) filtrate purifies: in step (1) gained filtrate, add copper sulfate 19.2g, under room temperature, stir lower purification 50 minutes, filter and be purified slag, its dry weight 9.6g(Sb0.07%, Cu47.77%); Scavenging solution 4.3L;
(3) scavenging solution oxidation: scavenging solution is warmed up to 97 ± 2 DEG C, add hydrogen peroxide (mass concentration is 30wt%) 245mL, oxidization time 50 minutes, filtration obtains wet sodium antimonate, be dried and obtain dry sodium antimonate 103.3g, its outward appearance is canescence, and main chemical compositions is: Sb47.97%, As0.02%, Fe0.04%, Cu0.05%, Pb0.02%; Alkali lye 5.4L after oxidation, its content NaOH252.0g/L, turns back to step (1) leaching stage, loops leaching.
In the present embodiment, the leaching yield 98.87% of antimony in antimony oxide ore; Leach, purify again to sodium antimonate from antimony oxide ore, the direct yield of its antimony is 92.89%; The rate of recovery of the copper in the mantoquita in scavenging agent is 60%.
Embodiment 5
The present embodiment comprises the following steps:
(1) antimony oxide ore leaches: antimony oxide ore is crushed to-150 orders, get-150 wherein Sb19.78%, As0.45%, Pb2.89%, Fe20.13% of object antimony oxide ore 500g(), add in 5.7L sodium hydroxide solution (NaOH concentration is 395.1g/L) and leach, add hydrazonium sulfate 29.7g, 90 ± 2 DEG C of extraction temperatures, extraction time 120 minutes; Then filter, obtain filter residue, dry rear wherein Sb0.41%, Fe30.66% of weight 325g(), wherein Sb18.67g/L of filtrate 5.2L();
(2) filtrate purifies: in step (1) gained filtrate, add cupric chloride 39.6g, under room temperature, stir lower purification 60 minutes, filter and be purified slag, its dry weight 24.7g(Sb0.06%, Cu49.10%) and scavenging solution 5.2L;
(3) scavenging solution oxidation: scavenging solution is warmed up to 90 ± 2 DEG C, add hydrogen peroxide (mass concentration is 30wt%) 485mL, oxidization time 60 minutes, filtration obtains wet sodium antimonate, be dried and obtain dry sodium antimonate 198.1g, its outward appearance is canescence, and main chemical compositions is: Sb48.00%, As0.08%, Fe0.03%, Cu0.01%, Pb0.02%; Alkali lye 6.5L after oxidation, its content NaOH312.0g/L, returns to step (1) and leaches, and recycles.
In the present embodiment, the leaching yield 98.65% of antimony in antimony oxide ore; Leach, purify again to sodium antimonate from antimony oxide ore, the direct yield of its antimony is 96.15%; The rate of recovery of the copper in the mantoquita in scavenging agent is 65%.
Described each embodiment, the antimony in antimony oxide ore and middle sample, arsenic, lead, iron, copper analytical procedure adopt YS/T239.1-2009 antimony concentrate chemical analysis method to carry out; Chemical composition analysis in sodium antimonate sample carries out according to YS/T22-2010 standard.
Claims (9)
1. antimony oxide ore alkaline process is prepared a method for sodium antimonate, it is characterized in that, comprises the following steps:
(1) antimony oxide ore leaches: antimony oxide ore is crushed to-150 orders, then leaches with sodium hydroxide solution, add reductive agent, maintenance temperature is 80-100 DEG C, and extraction time is 60-120 minute; Then filter, obtain filter residue and filtrate, filtrate is the sodium hydroxide solution containing antimony;
(2) filtrate purifies: in step (1) gained filtrate, add scavenging agent, the add-on of described scavenging agent is the 18-40% that is equivalent to antimony element mass content in feed oxygen antimony sulfide ore, and reaction 30-60 minute, filters, and filtrate is scavenging solution;
Described scavenging agent is water-soluble mantoquita;
(3) scavenging solution oxidation: add hydrogen peroxide to be oxidized toward step (2) gained scavenging solution at 60-100 DEG C, the add-on of described hydrogen peroxide be equivalent to antimony element quality in scavenging solution 3.0-5.0 doubly, maintenance temperature is 60-100 DEG C, reaction 30-60 minute, filters and obtains wet sodium antimonate and filtrate; By dry wet gained sodium antimonate, obtain product sodium antimonate; Regulate the concentration of sodium hydroxide in filtrate, return to step (1) and leach, recycle.
2. antimony oxide ore alkaline process according to claim 1 is prepared the method for sodium antimonate, it is characterized in that, in step (1), the composition of described antimony oxide ore is: antimony 10-20wt%, iron 10-20wt%, plumbous 1-3wt%, arsenic 0.1-0.5wt%.
3. antimony oxide ore alkaline process according to claim 1 and 2 is prepared the method for sodium antimonate, it is characterized in that, in step (1), the concentration that leaches sodium hydroxide used is 300-400g/L.
4. antimony oxide ore alkaline process according to claim 1 and 2 is prepared the method for sodium antimonate, it is characterized in that, in step (1), the liquid-solid ratio of described sodium hydroxide solution and antimony oxide ore is 10-16ml ︰ 1g.
5. antimony oxide ore alkaline process according to claim 3 is prepared the method for sodium antimonate, it is characterized in that, in step (1), the liquid-solid ratio of described sodium hydroxide solution and antimony oxide ore is 10-16ml ︰ 1g.
6. antimony oxide ore alkaline process according to claim 1 and 2 is prepared the method for sodium antimonate, it is characterized in that, in step (1), the add-on of reductive agent is the 14-30% that is equivalent to antimony element quality in antimony oxide ore.
7. the method for preparing sodium antimonate according to the antimony oxide ore alkaline process one of claim 1-6 Suo Shu, is characterized in that, in step (1), described reductive agent is hydrazine hydrate or hydrazonium sulfate.
8. the method for preparing sodium antimonate according to the antimony oxide ore alkaline process one of claim 1-7 Suo Shu, is characterized in that, in step (2), described scavenging agent is copper sulfate or cupric chloride.
9. the method for preparing sodium antimonate according to the antimony oxide ore alkaline process one of claim 1-8 Suo Shu, is characterized in that, in step (3), the concentration of described hydrogen peroxide is 27.5-60.0wt%.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106277052A (en) * | 2016-08-23 | 2017-01-04 | 陈安民 | A kind of stibium oxide produces the method for sodium antimonate |
| CN106480319A (en) * | 2016-10-26 | 2017-03-08 | 山东国大黄金股份有限公司 | A kind of method of the immersion cleaning treatment hydrogen containing tail gas synthetical recovery antimony of alkali containing antimony |
| CN107326188A (en) * | 2017-06-29 | 2017-11-07 | 郴州市金贵银业股份有限公司 | A kind of method for preparing sodium pyroantimonate with leaded silver-colored arsenic antimony cigarette ash |
| CN107858521A (en) * | 2017-12-07 | 2018-03-30 | 郴州市金贵银业股份有限公司 | The method that cigarette ash containing antimony prepares sodium pyroantimonate |
| CN108455669A (en) * | 2018-04-23 | 2018-08-28 | 长沙烨星锑业有限公司 | A kind of preparation method of schlippe's salt |
| KR20190052632A (en) * | 2017-11-08 | 2019-05-16 | 제일화학주식회사 | Method for preparing Sodium Antimonate |
| CN110343863A (en) * | 2019-07-23 | 2019-10-18 | 郴州市金贵银业股份有限公司 | A kind of method of alkali leaching separation antimony lead |
| CN112779425A (en) * | 2020-05-20 | 2021-05-11 | 昆明冶金研究院有限公司 | Method for preparing sodium antimonate from stibnite |
| CN113772726A (en) * | 2021-09-22 | 2021-12-10 | 长沙烨星锑业有限公司 | Preparation method for producing sodium antimonate by using ethylene glycol antimony distillation residues |
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| CN1408646A (en) * | 2001-09-25 | 2003-04-09 | 柳州市环东金属材料厂 | Process for producing sodium pyroantimonate |
| CN101693553A (en) * | 2009-10-19 | 2010-04-14 | 株洲安特锑业化工有限公司 | Production process for preparing ultra-white nanometer sodium pyroantimonate |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106277052A (en) * | 2016-08-23 | 2017-01-04 | 陈安民 | A kind of stibium oxide produces the method for sodium antimonate |
| CN106277052B (en) * | 2016-08-23 | 2018-02-06 | 陈安民 | A kind of method that sodium antimonate is produced with antimony oxide |
| CN106480319A (en) * | 2016-10-26 | 2017-03-08 | 山东国大黄金股份有限公司 | A kind of method of the immersion cleaning treatment hydrogen containing tail gas synthetical recovery antimony of alkali containing antimony |
| CN107326188A (en) * | 2017-06-29 | 2017-11-07 | 郴州市金贵银业股份有限公司 | A kind of method for preparing sodium pyroantimonate with leaded silver-colored arsenic antimony cigarette ash |
| CN107326188B (en) * | 2017-06-29 | 2019-03-08 | 郴州市金贵银业股份有限公司 | A method of sodium pyroantimonate is prepared with leaded silver-colored arsenic antimony cigarette ash |
| KR20190052632A (en) * | 2017-11-08 | 2019-05-16 | 제일화학주식회사 | Method for preparing Sodium Antimonate |
| KR102021997B1 (en) * | 2017-11-08 | 2019-09-18 | 제일화학주식회사 | Method for preparing Sodium Antimonate |
| CN107858521A (en) * | 2017-12-07 | 2018-03-30 | 郴州市金贵银业股份有限公司 | The method that cigarette ash containing antimony prepares sodium pyroantimonate |
| CN108455669A (en) * | 2018-04-23 | 2018-08-28 | 长沙烨星锑业有限公司 | A kind of preparation method of schlippe's salt |
| CN110343863A (en) * | 2019-07-23 | 2019-10-18 | 郴州市金贵银业股份有限公司 | A kind of method of alkali leaching separation antimony lead |
| CN112779425A (en) * | 2020-05-20 | 2021-05-11 | 昆明冶金研究院有限公司 | Method for preparing sodium antimonate from stibnite |
| CN113772726A (en) * | 2021-09-22 | 2021-12-10 | 长沙烨星锑业有限公司 | Preparation method for producing sodium antimonate by using ethylene glycol antimony distillation residues |
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