CN103866121B - A kind of antimony oxide ore alkaline process prepares the method for sodium antimonate - Google Patents
A kind of antimony oxide ore alkaline process prepares the method for sodium antimonate Download PDFInfo
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Abstract
Antimony oxide ore alkaline process prepares a method for sodium antimonate, comprises the steps: that (1) antimony oxide ore leaches; (2) filtrate purification; (3) scavenging solution oxidation.The rate of recovery of the present invention is high, the leaching yield of antimony is 95-99%, the direct yield of sodium antimonate is 90-95%, and whole process is carried out in alkaline environment, less demanding to equipment anticorrosion, 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.
Description
Technical field
The present invention relates to a kind of method preparing sodium antimonate, especially relate to a kind of method that antimony oxide ore alkaline process prepares 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 e.g., when the antimony grade in raw ore is below 10%, when obtaining 30% grade by ore dressing, its rate of recovery is about 50%; The antimony oxide ore of 10-20% is when by ore dressing, to bring up to grade be more than 30%, and its rate of recovery is about 60%; Therefore, the antimony oxide ore of general process 10-20%, the normal pyrogenic process that adopts carries out.If the antimony oxide ore of 10-20% grade is directly carried out straight well stove pyrometallurgical smelting, the evaporation rate of antimony is 50-60%; If by antimony oxide ore fine grinding to below 2mm, be mixed and made into cellular people's drum lump ore with coal, after drying, then carry out volatilization smelting in 900-1050 DEG C in straight well stove, its rate of recovery is 70-80%, and 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 when 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 prepares the method for sodium antimonate.
The technical scheme that the present invention solves the employing of its technical problem is that a kind of antimony oxide ore alkaline process prepares 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 is used for next procedure and purifies;
The composition of described antimony oxide ore is: antimony 10-20wt%, iron 10-20wt%, plumbous 1-3wt%, arsenic 0.1-0.5wt%;
(2) filtrate purification: add scavenging agent in step (1) gained filtrate, the add-on of described scavenging agent is the 18-40% being equivalent to antimony element mass content in material oxidation antimony ore, reaction 30-60 minute, filter, filtrate is scavenging solution; (adding scavenging agent makes the impurity element in leach liquor become precipitation, filters rear and solution separating)
Described scavenging agent is water-soluble mantoquita, preferably sulfuric acid copper or cupric chloride.
The object adding scavenging agent purifies the sulfocompound in leach liquor, and the existence of sulfocompound, affects the quality of the finished product, wherein mainly affects content and the outward appearance of principal constituent.Before preparing sodium antimonate, adopt mantoquita to purify to leach liquor, the sulfocompound in leach liquor and cupric ion generate the very little cupric sulfide of solubility product and separate.
(3) scavenging solution oxidation: add hydrogen peroxide toward step (2) gained scavenging solution and be oxidized at 60-100 DEG C, the add-on of described hydrogen peroxide is 3.0-5.0 times that is equivalent to antimony element quality in scavenging solution, maintenance temperature is 60-100 DEG C, reaction 30-60 minute, filters and obtains wet sodium antimonate and filtrate; Gained to be wet sodium antimonate drying, obtain product sodium antimonate; Regulate the concentration of sodium hydroxide in filtrate, return step (1) and leach, recycle.Whole process does not produce waste water.
Further, in step (1), the concentration leaching 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 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 dissolved in the sodium hydroxide solution of heat based on the antimonous oxide in antimony oxide ore, 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 the sodium hydroxide solution of heat, together leach.Its reaction formula is as follows:
The present invention adopts alkaline Leaching antimony oxide ore, and then, purification leach liquor, oxidation antimony wherein, obtain sodium antimonate, alkali lye returns leaching, recycles, the oxidized ore of this method process antimony, and the rate of recovery is high, does not pollute.
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 reached about 17%, adopt sodium hydroxide solution to leach, iron-based does not originally enter in solution, thus is isolated.The sodium antimonate that the present invention obtains is used as the finings of picture tube, opticglass and various high glass, the fire retardant of textiles, plastics, enamel opacifier, manufactures the composition of opaque filler that foundry goods paints and iron sheet, steel plate acid-proof varniss; For the identification of receiving ion in chemical analysis.
The rate of recovery of present method antimony is high, exceeds 30-35% than current pyrogenic processing method.Obtained by the present invention, sodium antimonate quality 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 object antimony oxide ore 100g(wherein Sb10.15wt%, As0.15wt%, Pb1.02wt%, Fe17.02wt%), add in 1.1L sodium hydroxide solution (NaOH concentration is 300.2g/L), add hydrazonium sulfate 1.5g, extraction temperature 82 ± 2 DEG C, extraction time 60 minutes; Then filter, obtain filter residue, weight 82g(wherein Sb0.51%, Fe20.55% after dry), filtrate 1.0L(wherein Sb9.73g/L);
(2) filtrate purification: add copper sulfate 2.0g in step (1) gained filtrate, under room temperature, stir 30 minutes, filters and is 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, drying obtains 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, its content NaOH245.2g/L, turns back to step (1) leaching stage, and circulation is leached.
In the present embodiment, the leaching yield 95.88% of antimony in antimony oxide ore; Leach from antimony oxide ore, purify again to sodium antimonate, 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 object antimony oxide ore 200g(wherein Sb16.45%, As0.25%, Pb2.51%, Fe16.73%), add 2.5L sodium hydroxide solution (NaOH content is 383.5g/L) to leach, add hydrazine hydrate 5.9g, extraction temperature 87 ± 2 DEG C, extraction time 70 minutes, then filter, obtain filter residue, weight 150g(wherein Sb0.33%, Fe22.15% after dry), filtrate 2.3L(wherein Sb14.21g/L);
(2) filtrate purification: add cupric chloride 8.2g in step (1) gained filtrate, under room temperature, stirs purification 35 minutes, filters 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, drying obtains 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, turn back to step (1) leaching stage, and circulation is leached.
In the present embodiment, the leaching yield 98.50% of antimony in antimony oxide ore; Leach from antimony oxide ore, purify again to sodium antimonate, 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 object antimony oxide ore 250g(wherein Sb13.59%, As0.35%, Pb2.68%, Fe18.79%), add in 3.4L sodium hydroxide solution (NaOH concentration is 358.9g/L), leach, add hydrazine hydrate 6.8g, extraction temperature 95 ± 2 DEG C, extraction time 90 minutes, then filters, obtains filter residue, weight 195g(wherein Sb0.56%, Fe23.85% after dry), filtrate 3.1L(wherein Sb10.65g/L);
(2) filtrate purification: add copper sulfate 10.2g in step (1) gained filtrate, under room temperature, stirs lower purification 45 minutes, filters 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, drying obtains 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, turn back to step (1) leaching stage, and circulation is leached.
In the present embodiment, the leaching yield 96.79% of antimony in antimony oxide ore; Leach from antimony oxide ore, purify again to sodium antimonate, 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 object antimony oxide ore 300g(wherein Sb17.78%, As0.28%, Pb1.86%, Fe10.45%), add in 4.7L sodium hydroxide solution (NaOH concentration is 334.6g/L) and leach, add hydrazine hydrate 13.3g, extraction temperature 82 ± 2 DEG C, extraction time 110 minutes, then filter, obtain filter residue, weight 216g(wherein Sb0.28%, Fe14.37% after dry), filtrate 4.3L(wherein Sb12.34g/L);
(2) filtrate purification: add copper sulfate 19.2g in step (1) gained filtrate, under room temperature, stirs lower purification 50 minutes, filters 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, drying obtains 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, turn back to step (1) leaching stage, and circulation is leached.
In the present embodiment, the leaching yield 98.87% of antimony in antimony oxide ore; Leach from antimony oxide ore, purify again to sodium antimonate, 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 object antimony oxide ore 500g(wherein Sb19.78%, As0.45%, Pb2.89%, Fe20.13%), add in 5.7L sodium hydroxide solution (NaOH concentration is 395.1g/L) and leach, add hydrazonium sulfate 29.7g, extraction temperature 90 ± 2 DEG C, extraction time 120 minutes; Then filter, obtain filter residue, weight 325g(wherein Sb0.41%, Fe30.66% after dry), filtrate 5.2L(wherein Sb18.67g/L);
(2) filtrate purification: add cupric chloride 39.6g in step (1) gained filtrate, under room temperature, stirs lower purification 60 minutes, filters 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, drying obtains 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, return step (1) and leach, recycle.
In the present embodiment, the leaching yield 98.65% of antimony in antimony oxide ore; Leach from antimony oxide ore, purify again to sodium antimonate, 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 (10)
1. antimony oxide ore alkaline process prepares 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 purification: add scavenging agent in step (1) gained filtrate, the add-on of described scavenging agent is the 18-40% being equivalent to antimony element mass content in material oxidation antimony ore, reaction 30-60 minute, filter, filtrate is scavenging solution;
Described scavenging agent is water-soluble mantoquita;
(3) scavenging solution oxidation: add hydrogen peroxide toward step (2) gained scavenging solution and be oxidized at 60-100 DEG C, the add-on of described hydrogen peroxide is 3.0-5.0 times that is equivalent to antimony element quality in scavenging solution, maintenance temperature is 60-100 DEG C, reaction 30-60 minute, filters and obtains wet sodium antimonate and filtrate; Gained to be wet sodium antimonate drying, obtain product sodium antimonate; Regulate the concentration of sodium hydroxide in filtrate, return step (1) and leach, recycle;
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%;
In step (1), described reductive agent is hydrazine hydrate or hydrazonium sulfate.
2. antimony oxide ore alkaline process according to claim 1 prepares the method for sodium antimonate, it is characterized in that, in step (1), the concentration leaching sodium hydroxide used is 300-400g/L.
3. antimony oxide ore alkaline process according to claim 1 and 2 prepares 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.
4. antimony oxide ore alkaline process according to claim 1 and 2 prepares the method for sodium antimonate, it is characterized in that, in step (1), the add-on of reductive agent is the 14-30% being equivalent to antimony element quality in antimony oxide ore.
5. antimony oxide ore alkaline process according to claim 1 and 2 prepares the method for sodium antimonate, it is characterized in that, in step (2), described scavenging agent is copper sulfate or cupric chloride.
6. antimony oxide ore alkaline process according to claim 3 prepares the method for sodium antimonate, it is characterized in that, in step (2), described scavenging agent is copper sulfate or cupric chloride.
7. antimony oxide ore alkaline process according to claim 4 prepares the method for sodium antimonate, it is characterized in that, in step (2), described scavenging agent is copper sulfate or cupric chloride.
8. antimony oxide ore alkaline process according to claim 1 and 2 prepares the method for sodium antimonate, it is characterized in that, in step (3), the concentration of described hydrogen peroxide is 27.5-60.0wt%.
9. antimony oxide ore alkaline process according to claim 3 prepares the method for sodium antimonate, it is characterized in that, in step (3), the concentration of described hydrogen peroxide is 27.5-60.0wt%.
10. antimony oxide ore alkaline process according to claim 4 prepares the method for sodium antimonate, it is characterized in that, in step (3), the concentration of described hydrogen peroxide is 27.5-60.0wt%.
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| 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 |
| 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 |
| 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 |
| CN110343863B (en) * | 2019-07-23 | 2021-06-25 | 郴州市金贵银业股份有限公司 | Method for separating antimony and lead by alkaline leaching |
| 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 |
| CN113772726B (en) * | 2021-09-22 | 2023-06-06 | 长沙烨星锑业有限公司 | Preparation method for producing sodium antimonate by using glycol antimony distilled slag |
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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 |
| CN102680470B (en) * | 2011-12-10 | 2014-04-02 | 河南科技大学 | Method for determining content of arsenic and antimony in copper electrolyte |
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