CN110054213A - A method of sodium stannate is prepared using high-silicon type cassiterite concentrate soda roasting - Google Patents
A method of sodium stannate is prepared using high-silicon type cassiterite concentrate soda roasting Download PDFInfo
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Abstract
The invention discloses a kind of methods for preparing sodium stannate using high silicon cassiterite concentrate soda roasting, pass through the roasting conditions such as control two-stage roasting process ratio sodium carbonate, maturing temperature, atmosphere, regulate and control the reaction in soda roasting process between stannic oxide, silica and sodium carbonate, inhibit the formation of sodium silicon tin ternary oxide, promote the generation of sodium stannate simultaneously, the final conversion ratio for improving sodium stannate, the tin rate of recovery is improved to 98.6% or more.
Description
Technical field
It is the present invention relates to a kind of method for preparing diluted acid sodium using high-silicon type cassiterite concentrate, in particular to a kind of using secondary
The method that roasting technique improves sodium stannate yield in cassiterite concentrate soda roasting process belongs to non-ferrous metal metallurgy and chemical industry neck
Domain.
Background technique
Sodium stannate is the most commonly used a kind of tin heavy chemicals of purposes, is applied to multiple necks such as plating, dyestuff, material processing
Domain.The main preparation methods of sodium stannate include alkali analysis method and stripping method, mainly using metallic tin as raw material and sodium hydroxide and oxidation
Agent reaction, is prepared into sodium stannate solution, then is cleaned, crystallization and purification, separation crystallization acquisition product.Traditional sodium stannate preparation
Process costs are high, low yield, the high requirements on the equipment.
Cassiterite concentrate soda roasting method is using cassiterite concentrate as raw material, with addition of sodium salts such as sodium carbonate, in the effect of reducing agent
The lower formation for promoting sodium stannate is obtaining sodium stannate product by leaching, removal of impurities, purification, separation process, which easily obtains
It obtains, simple process, low production cost.But original tin is mostly close with the gangue minerals such as quartz, garnet, calcite
Association, symbiosis are continuously improved by multistage " mill-choosing " tin grade, but still contain a certain proportion of gangue mine in cassiterite concentrate
Object, especially quartz content are higher.Cassiterite concentrate passes through oxidizing roasting acidleach two-step method technique, can substantially remove
The impurity such as sulphur, arsenic, lead, zinc, constituent content are respectively less than 0.005%；But prior art can not remove the dioxy in cassiterite concentrate
SiClx, dioxide-containing silica is generally 10% or more in concentrate.
Silica is a kind of acidic oxide that property is stable, and in the presence of having sodium salt, temperature is higher than 700
DEG C when, be just easy to reaction generate low melting point sodium metasilicate；And in cassiterite concentrate soda roasting process, silica and tin
Stone, sodium carbonate are also being easy to happen combination reaction, generate silicon-tin-sodium ternary oxide, this ternary oxide fusing point is only
700 DEG C or so, tight is on cassiterite surface, it is suppressed that the generation of sodium stannate is reacted.In addition, sodium silicon tin ternary oxide is insoluble
In weak acid, aqueous slkali, in subsequent leaching process, the leaching rate of recovery of tin is greatly reduced, therefore, existing cassiterite concentrate soda
Roasting is prepared in sodium stannate technique, the conversion ratio of tin be only 85% or so (patent No. ZL201210412835.9,
ZL201210411593.1), part tin is remained in leached mud in the form of sodium silicon tin ternary oxide, causes the wave of tin resource
Take.
Summary of the invention
To solve to prepare in sodium stannate technical process using high silicon cassiterite concentrate as material soda roasting, silica is to stannic acid
The adverse effects such as the conversion of sodium stannate caused by sodium the generates rate of recovery is low, tin loss is big, the purpose of the invention is to provide one
Kind using secondary reduction roasting technique inhibit high-silicon type cassiterite concentrate soda roasting process in sodium silicon tin ternary oxide generate with
The conversion ratio for improving sodium stannate, the method for reducing tin loss, this method is easy to operate, production cost is low, environmental-friendly, meets work
Industry production requirement.
In order to achieve the above technical purposes, stannic acid is prepared using high silicon cassiterite concentrate soda roasting the present invention provides a kind of
The method of sodium comprising following steps:
1) by high silicon cassiterite concentrate and sodium carbonate according to Na:(Sn+Si) to be that 2.1:1~2.6:1 is carried out primary for molar ratio
Ingredient, after mixing, being levigate, agglomeration, drying, then it is placed in CO-CO2One is carried out in 750~850 DEG C of roasting temperatures in mixed atmosphere
Secondary roasting, product of roasting is crushed after supercooling, then is placed in sodium hydroxide solution and is carried out mill leaching, is separated by solid-liquid separation, is obtained stannic acid
Sodium solution and a leached mud；Wherein, CO-CO2Carbon monoxide volume ratio is 10~15% in mixed atmosphere；
2) leached mud and sodium carbonate being carried out according to Na:(Sn+Si) to be that 3:1~3.5:1 is carried out secondary for molar ratio
Ingredient, after mixing, being levigate, agglomeration, drying, then it is placed in CO-CO2Two are carried out in 750~850 DEG C of roasting temperatures in mixed atmosphere
Secondary roasting, product of roasting is crushed after supercooling, then is placed in sodium hydroxide solution and is carried out mill leaching, is separated by solid-liquid separation, is obtained stannic acid
Sodium solution and secondary leached mud；Wherein, CO-CO2Carbon monoxide volume ratio is 5~10% in mixed atmosphere；
3) by step 1) and 2) in sodium stannate solution together by concentration and fractional crystallization, obtain sodium stannate.
Preferred scheme, the high silicon cassiterite concentrate is by oxidizing roasting-acidleach removal of impurities pretreatment.High silicon cassiterite concentrate is pre-
Oxidizing roasting conventional in the prior art-acidleach removal of impurities is first passed through, the impurity contents such as iron, calcium, aluminium, magnesium can be lower than
0.01%, remaining major impurity is silica, and content is higher than 8%.
Preferred scheme, high silicon cassiterite concentrate and sodium carbonate mix and levigate are less than 0.1mm to granularity 100%.In advance will
Raw material is all ground to appropriate granularity, it is ensured that the good contact between material particles makes solid phase reaction in roasting process can
With smooth, quick progress.
Preferred scheme, the time once roasted are 30~60min.
Preferred scheme, leached mud and sodium carbonate mix and levigate are less than 0.1mm to granularity 100%.
Preferred scheme, the time of the after baking are 30~60min.
Preferred scheme, step 1) and 2) in sodium hydroxide solution pH value be 10.5~12.5.
Separation of solid and liquid process of the invention can be separated by filtration for conventional.
Concentration and fractional crystallization process of the invention is the routine operation of this field.
In order to achieve the above technical purposes, provided by the invention to prepare sodium stannate using the soda roasting of high-silicon type cassiterite concentrate
Method, comprising the following specific steps
1) by high silicon cassiterite concentrate and sodium carbonate according to Na:(Sn+Si) to be that 2.1:1~2.6:1 is carried out primary for molar ratio
Ingredient, mixing, it is levigate to 100% be less than -0.1mm after agglomeration, drying, be subsequently placed in CO-CO2Roasting carries out one section of roasting in atmosphere
Burn, maturing temperature is 750~850 DEG C, 30~60min of calcining time, in calcination atmosphere carbon monoxide volume ratio be 10~
15%；After roasting, material after cooling is broken, sodium hydroxide solution (sodium hydroxide solution pH value is 10.5~
12.5) mill leaching is carried out in, is then separated by filtration and is obtained sodium stannate solution and a leached mud；
2) by a leached mud and sodium carbonate according to Na:(Sn+Si) molar ratio be 3:1~3.5:1 carry out second batch,
Mix, it is levigate to 100% be less than -0.1mm after agglomeration, drying, be subsequently placed in CO-CO2Roasting progress two-stage calcination in atmosphere, two
Secondary maturing temperature is 750~800 DEG C, 30~60min of calcining time, and carbon monoxide volume ratio is 5~10% in calcination atmosphere
After roasting, material after cooling is crushed, in sodium hydroxide solution (sodium hydroxide solution pH value is 10.5~12.5)
Mill leaching is carried out, is then separated by filtration and obtains sodium stannate solution and secondary leached mud；
3) after two-stage roasting-mill leaching, sodium stannate solution passes through concentration, fractional crystallization, is separated by filtration acquisition sodium stannate twice
Product.
In the prior art in high-silicon type cassiterite concentrate soda roasting process, sodium metasilicate binary chemical combination inevitably will form
Object and sodium silicon tin ternary oxide, two substances are low-melting-point material, form partial liquid phase in roasting process, are wrapped in cassiterite
Particle surface inhibits subsequent reactions to carry out.In addition, the extremely difficult dissolution under alkalescent system of sodium silicon tin ternary oxide, is unfavorable for
The separation and recovery of tin is the main reason for causing soda roasting process tin to lose.Technical solution of the present invention key is to high silicon
Sodium silicon tin element ratio carries out Effective Regulation in cassiterite concentrate and sodium carbonate mixed raw material, and combines multistage roasting process temperature
Optimize with atmosphere, have been surprisingly found that, sodium silicon tin ternary in high-silicon type cassiterite concentrate soda roasting process can be inhibited to aoxidize well
The production of object, promotes the generation of sodium stannate, to improve the conversion ratio of sodium stannate, realizes the high efficiente callback of tin element.
Compared with the prior art, technical solution of the present invention bring the utility model has the advantages that
1) technical solution of the present invention is remarkably improved the conversion ratio of cassiterite concentrate soda roasting process sodium stannate, and tin is comprehensive
The rate of recovery is increased to 98.6% or more.
2) technical solution of the present invention passes through regulation two-stage roasting process sodium carbonate amount, maturing temperature and atmosphere lamp ginseng
Number realizes the formation for inhibiting sodium silicon tin ternary oxide, while promoting the conversion of sodium stannate, does not use other additives and price
Expensive Organic Sodium Salt etc., reduces production cost.
3) technical solution of the present invention is easy to operate, low energy consumption, at low cost, it is easy to accomplish industrialized production.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
Following embodiment is intended to further illustrate the content of present invention, rather than limits the protection model of the claims in the present invention
It encloses.
Embodiment 1:
With cassiterite concentrate, (Sn content is 70.0%, SiO2Content is 11.7%) and sodium carbonate (analysis pure) is raw material, and one
Section ingredient according to Na:(Sn+Si) ratio be 2.5:1, after mixing it is levigate to 100% be less than -0.1mm, agglomeration later, drying, into
One section of row roasting, 850 DEG C of maturing temperature, calcining time 60min, CO content is 15% in calcination atmosphere, by object after roasting
Material is broken, and leaching is ground in the sodium hydroxide solution that pH is 12.5, and filtering obtains sodium stannate solution and a leached mud；Then will
Leached mud and sodium carbonate carry out second batch, according to Na:(Sn+Si) ratio is 3.1:1, it is levigate after mixing be less than to 100%-
0.1mm, agglomeration later, drying carry out two-stage calcination, 750 DEG C of maturing temperature, calcining time 30min, CO content in calcination atmosphere
It is 5%, is crushed material after roasting, and grind leaching in the sodium hydroxide solution that pH is 10.5, it is molten that filtering obtains sodium stannate
Liquid and secondary leached mud will separate twice and obtain the processing such as sodium stannate leachate, purification and impurity removal, condensing crystallizing, and obtain sodium stannate
Product.The rate of recovery of tin is 98.6%.
Embodiment 2:
With cassiterite concentrate, (Sn content is 70.0%, SiO2Content is 11.7%) and sodium carbonate (analysis pure) is raw material, and one
Section ingredient according to Na:(Sn+Si) ratio be 2.1:1, after mixing it is levigate to 100% be less than -0.1mm, agglomeration later, drying, into
One section of row roasting, 750 DEG C of maturing temperature, calcining time 30min, CO content is 10% in calcination atmosphere, by object after roasting
Material is broken, and leaching is ground in the sodium hydroxide solution that pH is 11.5, and filtering obtains sodium stannate solution and a leached mud；Then will
Leached mud and sodium carbonate carry out second batch, according to Na:(Sn+Si) ratio is 3.5:1, it is levigate after mixing be less than to 100%-
0.1mm, agglomeration later, drying carry out two-stage calcination, 800 DEG C of maturing temperature, calcining time 60min, CO content in calcination atmosphere
It is 10%, is crushed material after roasting, and grind leaching in the sodium hydroxide solution that pH is 10.5, it is molten that filtering obtains sodium stannate
Liquid and secondary leached mud will separate twice and obtain the processing such as sodium stannate leachate, purification and impurity removal, condensing crystallizing, and obtain sodium stannate
Product.The rate of recovery of tin is 99.3%.
Embodiment 3:
With cassiterite concentrate, (Sn content is 72.0%, SiO2Content is 8.1%) and sodium carbonate (analysis pure) is raw material, and one section
Ingredient is according to Na:(Sn+Si) ratio be 2.5:1, after mixing it is levigate to 100% be less than -0.1mm, agglomeration later, drying, carry out
One section of roasting, 795 DEG C of maturing temperature, calcining time 45min, CO content is 10.5% in calcination atmosphere, by object after roasting
Material is broken, and leaching is ground in the sodium hydroxide solution that pH is 11.5, and filtering obtains sodium stannate solution and a leached mud；Then will
Leached mud and sodium carbonate carry out second batch, according to Na:(Sn+Si) ratio is 3.2:1, it is levigate after mixing be less than to 100%-
0.1mm, agglomeration later, drying carry out two-stage calcination, 825 DEG C of maturing temperature, calcining time 60min, CO content in calcination atmosphere
It is 10%, is crushed material after roasting, and grind leaching in the sodium hydroxide solution that pH is 12.5, it is molten that filtering obtains sodium stannate
Liquid and secondary leached mud will separate twice and obtain the processing such as sodium stannate leachate, purification and impurity removal, condensing crystallizing, and obtain sodium stannate
Product.The rate of recovery of tin is 99.2%.
Embodiment 4:
With cassiterite concentrate, (Sn content is 72.0%, SiO2Content is 8.1%) and sodium carbonate (analysis pure) is raw material, and one section
Ingredient is according to Na:(Sn+Si) ratio be 2.2:1, after mixing it is levigate to 100% be less than -0.1mm, agglomeration later, drying, carry out
One section of roasting, 850 DEG C of maturing temperature, calcining time 30min, CO content is 13.5% in calcination atmosphere, by object after roasting
Material is broken, and leaching is ground in the sodium hydroxide solution that pH is 10.5, and filtering obtains sodium stannate solution and a leached mud；Then will
Leached mud and sodium carbonate carry out second batch, according to Na:(Sn+Si) ratio is 3.2:1, it is levigate after mixing be less than to 100%-
0.1mm, agglomeration later, drying carry out two-stage calcination, 775 DEG C of maturing temperature, calcining time 30min, CO content in calcination atmosphere
It is 10%, is crushed material after roasting, and grind leaching in the sodium hydroxide solution that pH is 10.5, it is molten that filtering obtains sodium stannate
Liquid and secondary leached mud will separate twice and obtain the processing such as sodium stannate leachate, purification and impurity removal, condensing crystallizing, and obtain sodium stannate
Product.The rate of recovery of tin is 99.0%.
Comparative example 1
With cassiterite concentrate, (Sn content is 72.0%, SiO2Content is 8.1%) and sodium carbonate (analysis is pure) is raw material, ingredient
According to Na:(Sn+Si) ratio is 2.2:1, levigate after mixing to be less than -0.1mm to 100%, agglomeration later, drying roasted,
850 DEG C of maturing temperature, calcining time 60min, CO content is 13.5% in calcination atmosphere, is crushed material after roasting, and
Leaching is ground in the sodium hydroxide solution that pH is 10.5, filtering obtains sodium stannate solution and secondary leached mud, will separate acquisition twice
The processing such as sodium stannate leachate, purification and impurity removal, condensing crystallizing, obtains sodium stannate product.The rate of recovery of tin is 74.0%.
Comparative example 2:
With cassiterite concentrate, (Sn content is 70.0%, SiO2Content is 11.7%) and sodium carbonate (analysis pure) is raw material, and one
Section ingredient according to Na:(Sn+Si) ratio be 2.5:1, after mixing it is levigate to 100% be less than -0.1mm, agglomeration later, drying, into
One section of row roasting, 850 DEG C of maturing temperature, calcining time 60min, calcination atmosphere are air, are crushed material after roasting, and
Leaching is ground in the sodium hydroxide solution that pH is 12.5, filtering obtains sodium stannate solution and a leached mud；Then by leached mud with
Sodium carbonate carry out second batch, according to Na:(Sn+Si) ratio be 3.1:1, after mixing it is levigate to 100% be less than -0.1mm, later
Agglomeration, drying carry out two-stage calcination, and 750 DEG C of maturing temperature, calcining time 30min, calcination atmosphere are air, after roasting
Material is crushed, and grinds leaching in the sodium hydroxide solution that pH is 10.5, filtering obtains sodium stannate solution and secondary leached mud, will
Separation twice obtains the processing such as sodium stannate leachate, purification and impurity removal, condensing crystallizing, obtains sodium stannate product.The rate of recovery of tin is
53.2%.
Comparative example 3:
With cassiterite concentrate, (Sn content is 70.0%, SiO2Content is 11.7%) and sodium carbonate (analysis pure) is raw material, and one
Section ingredient according to Na:(Sn+Si) ratio be 2.5:1, after mixing it is levigate to 100% be less than -0.1mm, agglomeration later, drying, into
One section of row roasting, 850 DEG C of maturing temperature, calcining time 60min, CO content is 35% in calcination atmosphere, by object after roasting
Material is broken, and leaching is ground in the sodium hydroxide solution that pH is 12.5, and filtering obtains sodium stannate solution and a leached mud；Then will
Leached mud and sodium carbonate carry out second batch, according to Na:(Sn+Si) ratio is 3.1:1, it is levigate after mixing be less than to 100%-
0.1mm, agglomeration later, drying carry out two-stage calcination, 750 DEG C of maturing temperature, calcining time 30min, CO content in calcination atmosphere
It is 2.5%, is crushed material after roasting, and grind leaching in the sodium hydroxide solution that pH is 10.5, filtering obtains sodium stannate
Solution and secondary leached mud will separate twice and obtain the processing such as sodium stannate leachate, purification and impurity removal, condensing crystallizing, and obtain stannic acid
Sodium product.The rate of recovery of tin is 34.2%.
Comparative example 4:
With cassiterite concentrate, (Sn content is 70.0%, SiO2Content is 11.7%) and sodium carbonate (analysis pure) is raw material, and one
Section ingredient according to Na:(Sn+Si) ratio be 2.0:1, after mixing it is levigate to 100% be less than -0.1mm, agglomeration later, drying, into
One section of row roasting, 850 DEG C of maturing temperature, calcining time 60min, CO content is 15% in calcination atmosphere, by object after roasting
Material is broken, and leaching is ground in the sodium hydroxide solution that pH is 12.5, and filtering obtains sodium stannate solution and a leached mud；Then will
Leached mud and sodium carbonate carry out second batch, according to Na:(Sn+Si) ratio is 3.0:1, it is levigate after mixing be less than to 100%-
0.1mm, agglomeration later, drying carry out two-stage calcination, 750 DEG C of maturing temperature, calcining time 30min, CO content in calcination atmosphere
It is 5%, is crushed material after roasting, and grind leaching in the sodium hydroxide solution that pH is 10.5, it is molten that filtering obtains sodium stannate
Liquid and secondary leached mud will separate twice and obtain the processing such as sodium stannate leachate, purification and impurity removal, condensing crystallizing, and obtain sodium stannate
Product.The rate of recovery of tin is 60.8%.
Claims (7)
1. a kind of method for preparing sodium stannate using high silicon cassiterite concentrate soda roasting, it is characterised in that: the following steps are included:
1) by high silicon cassiterite concentrate and sodium carbonate according to Na:(Sn+Si) molar ratio be 2.1:1~2.6:1 carry out Primary batching system,
After mixing, being levigate, agglomeration, drying, then it is placed in CO-CO2It is once roasted in mixed atmosphere in 750~850 DEG C of roasting temperatures
It burns, product of roasting is crushed after supercooling, then is placed in sodium hydroxide solution and is carried out mill leaching, is separated by solid-liquid separation, it is molten to obtain sodium stannate
Liquid and a leached mud；Wherein, CO-CO2Carbon monoxide volume ratio is 10~15% in mixed atmosphere；
2) leached mud and sodium carbonate being carried out according to Na:(Sn+Si) molar ratio is that 3:1~3.5:1 carries out second batch,
After mixing, being levigate, agglomeration, drying, then it is placed in CO-CO2Secondary roasting is carried out in 750~850 DEG C of roasting temperatures in mixed atmosphere
It burns, product of roasting is crushed after supercooling, then is placed in sodium hydroxide solution and is carried out mill leaching, is separated by solid-liquid separation, it is molten to obtain sodium stannate
Liquid and secondary leached mud；Wherein, CO-CO2Carbon monoxide volume ratio is 5~10% in mixed atmosphere；
3) by step 1) and 2) in sodium stannate solution together by concentration and fractional crystallization, obtain sodium stannate.
2. a kind of method for preparing sodium stannate using high silicon cassiterite concentrate soda roasting according to claim 1, feature
Be: the high silicon cassiterite concentrate is by oxidizing roasting-acidleach removal of impurities pretreatment.
3. a kind of method for preparing sodium stannate using high silicon cassiterite concentrate soda roasting according to claim 1, feature
Be: high silicon cassiterite concentrate and sodium carbonate mix and levigate are less than 0.1mm to granularity 100%.
4. a kind of method for preparing sodium stannate using high silicon cassiterite concentrate soda roasting according to claim 1, feature
Be: the time once roasted is 30~60min.
5. a kind of method for preparing sodium stannate using high silicon cassiterite concentrate soda roasting according to claim 1, feature
Be: leached mud and sodium carbonate mix and levigate are less than 0.1mm to granularity 100%.
6. a kind of method for preparing sodium stannate using high silicon cassiterite concentrate soda roasting according to claim 1, feature
Be: the time of the after baking is 30~60min.
7. a kind of method for preparing sodium stannate using high silicon cassiterite concentrate soda roasting according to claim 1, feature
Be: step 1) and 2) in sodium hydroxide solution pH value be 10.5~12.5.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BG33057A1 (en) * | 1981-11-24 | 1982-12-15 | Maneva | Method for obtaining of sodium stannate |
| CN102923764A (en) * | 2012-10-25 | 2013-02-13 | 中南大学 | Method for preparing sodium stannate from stannic oxide and sodium salt in reduction roasting manner |
| CN104152675A (en) * | 2014-07-21 | 2014-11-19 | 中南大学 | Method for preparing metallic tin and sodium silicate by utilizing high-silicon type cassiterite concentrate |
-
2019
- 2019-04-25 CN CN201910338893.3A patent/CN110054213B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BG33057A1 (en) * | 1981-11-24 | 1982-12-15 | Maneva | Method for obtaining of sodium stannate |
| CN102923764A (en) * | 2012-10-25 | 2013-02-13 | 中南大学 | Method for preparing sodium stannate from stannic oxide and sodium salt in reduction roasting manner |
| CN104152675A (en) * | 2014-07-21 | 2014-11-19 | 中南大学 | Method for preparing metallic tin and sodium silicate by utilizing high-silicon type cassiterite concentrate |
Non-Patent Citations (3)
| Title |
|---|
| WANG LICHUAN等: "DIRECT PREPAPRATION OF SODIUM STANNATE FROM TIN CONCENTRATES", 《J.CENT-SOUTH INST. MIN. METALL》 * |
| 张元波等: "二氧化锡钠盐焙烧-水浸制备锡酸钠的可行性研究", 《矿冶工程》 * |
| 杨光: "锡石精矿苏打焙烧-浸出制备锡酸钠的研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
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