CN100560500C - The preparation method of high-quality strontium carbonate - Google Patents
The preparation method of high-quality strontium carbonate Download PDFInfo
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- CN100560500C CN100560500C CN 200710018051 CN200710018051A CN100560500C CN 100560500 C CN100560500 C CN 100560500C CN 200710018051 CN200710018051 CN 200710018051 CN 200710018051 A CN200710018051 A CN 200710018051A CN 100560500 C CN100560500 C CN 100560500C
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- strontium carbonate
- strontium
- carbonate powder
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- sulfide solution
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Abstract
The invention provides a kind of is the novel method of raw material production Strontium carbonate powder with the celestite ore, and this method gets strontium sulfide solution with grey black water counter-current extraction again with lazurite breeze and the baking mixed in certain proportion grey black that obtains of reduction coal dust; With soda ash is carburization agent, under agitation in 90～100 ℃ of reactions 0.5～5 hour, generates and contains the Strontium carbonate powder precipitation and hang down the slip of iron Gas with Sodium Sulfide Solution, obtains the Strontium carbonate powder precipitation and hangs down the iron Gas with Sodium Sulfide Solution by solid-liquid separation; Strontium carbonate powder water countercurrent washing 3～5 times, drying obtains the high-quality strontium carbonate product; The mother liquor first time of washing Strontium carbonate powder merges with the centrifuge mother liquor of Strontium carbonate powder slip, by being the vacuum-evaporator evaporation of medium with the thermal oil, obtains hanging down iron Sodium Sulphide byproduct.Production technique of the present invention is simplified, and flow process is short, cost is low, and facility investment is little, and the quality height of major and minor product has good economic benefits.
Description
Technical field
The invention belongs to chemical field, relate to a kind of high-quality strontium carbonate preparation method, relating in particular to a kind of is the method for raw material production high-quality strontium carbonate product with the celestite ore.
Background technology
Strontium carbonate powder is topmost strontium product salt, is mainly used in to produce color monitor glass bulb, magneticsubstance, pyrotechnics etc., and Application Areas relates to electronics, material, chemical industry, sugaring, metallurgy, military project etc.The production technique of Strontium carbonate powder mainly comprises grey black method (being carbon reduction method) and double decomposition, but because double decomposition need consume a large amount of Chemicals (acid, alkali, salt etc.), technical process is long, and product purity is lower, the more high shortcoming of cost seldom adopts in industrial production.The grey black method is by become the strontium sulfide of solubility with coal reduction celestite ore, take out the strontium sulfide of solubility then by water logging, remove barium (for high barytocelestite ore deposit) by sulfuric acid, the carbon dioxide carbonization that obtains with the coal calcination Wingdale obtains Strontium carbonate powder again.This method often has elemental sulfur to be present in the strontium carbonate product in producing, cause the strontium carbonate product quality to descend, produce more elemental sulfur in some production process, can in precipitation process, drag for floating sulphur, but this method can not guarantee the stable of quality product and produce qualified strontium carbonate product.Elemental sulfur is formed at the celestite ore reduction phase, because the control of CARBON REDUCTION PROCESS OF TANTALUM processing condition is improper, make reduction intermediate product elemental sulfur form in a large number, and elemental sulfur forms many strontium sulfides and enters solution with strontium sulfide in the process of leaching strontium sulfide, when with the carbonic acid gas carbonization, elemental sulfur parses and enters in the strontium carbonate product, causes the Strontium carbonate powder quality to descend.
Chinese patent CN01108658.0 disclosed " a kind of reprocessing cycle is produced the method for Strontium carbonate powder " is with the by product carbonic acid gas of celestite powder and coal roasting generation and the by product sodium sulphite reaction of strontium sulfide and soda ash reaction, resynthesis soda ash, circulation repeatedly.Because the carbon dioxide of by-product contains more impurity and solid micronic dust in the CARBON REDUCTION PROCESS OF TANTALUM, make to become cumbersome, and the quality of synthetic soda ash is not necessarily suited for producing the demand of Strontium carbonate powder with the synthetic soda ash of sodium sulphite mother liquor reaction.
Summary of the invention
It is raw material with the celestite ore that purpose of the present invention provides a kind of, adopt calcined soda for industry to produce the novel method of Strontium carbonate powder as carburization agent.
The present invention produces the method for high-quality strontium carbonate product, comprises following processing step:
1. the lazurite breeze is mixed with the part by weight of reduction coal dust with 1: 0.5～1: 5, obtained grey black in 0.5～10 hour, again grey black water counter-current extraction is got strontium sulfide solution at 900～1300 ℃ roasting temperatures; The strontium sulfide solution concentration of leaching is controlled at 100～250g/L; The carbon reduction lazurite generally adopts the rotary kiln continuous production, and wherein to select Strontium Sulphate content for use be 55～75% lazurite breeze to lazurite; Also raw coal is for can select coking coal, non-caking coal, lean coal, bottle coal, rich coal for use, and long-flame coal, hard coal etc. are any;
2. the soda ash that adds strontium sulfide molar weight 95～105% under agitation in 90～100 ℃ of reactions 0.5～5 hour, generates and contains the Strontium carbonate powder precipitation and hang down the slip of iron Gas with Sodium Sulfide Solution; Wherein soda ash can adopt calcined soda for industry solution or solid soda ash, and liquid soda ash can adopt header tank to be metered into, and solid soda ash can add continuously by feeding screw;
3. slip is obtained the Strontium carbonate powder precipitation and hangs down the iron Gas with Sodium Sulfide Solution by centrifugation;
4. with Strontium carbonate powder water countercurrent washing 3～5 times, drying obtains the high-quality strontium carbonate product; The mother liquor first time of washing Strontium carbonate powder is merged with the low iron Gas with Sodium Sulfide Solution that 3. step obtains,, obtain hanging down iron Sodium Sulphide byproduct by being the vacuum-evaporator evaporation of medium with the thermal oil.
The key that reduces sulphur content in the Strontium carbonate powder is to control well the processing condition of reduction process, makes reduction process carry out fully, reduce the formation of reduction process intermediate product elemental sulfur, but this is relatively more difficult sometimes in scale operation.The elemental sulfur that generates in the CARBON REDUCTION PROCESS OF TANTALUM generates many strontium sulfides with the strontium sulfide reaction in using the process of water extraction, this many strontium sulfides make the leach liquor of strontium sulfide present yellow, so be commonly called as yellow water.The chemical reaction of strontium sulfide leaching process is:
SrS+(x-1)S→SrS
x
With soda ash carbonization yellow water, many strontium sulfides are converted into sodium polysulphide and enter carbonization mother liquor, do not parse elemental sulfur, and the sulphur content in the Strontium carbonate powder can greatly reduce.When reclaiming Sodium Sulphide from mother liquor, sodium polysulphide enters in the Sodium Sulphide product, but does not influence the quality of sodium sulphite product, and iron level is very low in the Sodium Sulphide that reclaims, and belongs to low iron Sodium Sulphide, and the market requirement is vigorous.Following reaction takes place in the soda ash carbonization:
SrS
x+Na
2CO
3→SrCO
3+Na
2S
x(x＞1)
In this method, by soda ash amount control techniques and special Strontium carbonate powder washing methods, the integrated quality of the strontium carbonate product of preparation is had greatly improved, resulting strontium carbonate product is carried out GB GB10660-1989 analytical procedure, and the every index of product is as follows:
Strontium carbonate powder (SrCO
3) content 〉=97.0%, lime carbonate (CaCO
3) content≤0.50%, barium carbonate (BaCO
3) content≤1.0%, sodium (Na) content≤0.25%, iron is (with Fe
2O
3Meter) content≤0.01%, muriate (in Cl) content≤0.12%, total sulfur (in S) content≤0.08%, phosphorus is (with P
2O
5Meter) content≤0.01%, moisture≤0.3%, hydrochloric acid insoluble substance content≤0.15% all is better than the technical requirements of GB top grade product.
The low iron Sodium Sulphide of by product Containing Sulfur sodium 60～70% of the present invention is carried out GB GB/T 10500-2000 analytical procedure, and product reaches the technical indicator of low iron Sodium Sulphide: sodium sulphite (Na
2S) content 〉=60%, S-WAT (Na
2SO
3) content≤2.0%, Sulfothiorine (Na
2S
2O
3) content≤2.0%, total iron (in Fe) content≤0.003%, water insoluble matter content≤0.1%.
The present invention compared with prior art has the following advantages:
1, the present invention is raw material with the celestite ore, adopts calcined soda for industry as carburization agent, make many strontium sulfides be converted into sodium polysulphide and enter carbonization mother liquor, do not parse elemental sulfur, sulphur content in the Strontium carbonate powder can greatly reduce, improved the integrated quality of Strontium carbonate powder, made every technical indicator of strontium carbonate product all be better than the high-quality of industrial premium grads.
2, the present invention is by reclaiming the low iron Sodium Sulphide in the mother liquor, the comprehensive cost that makes this technology produce Strontium carbonate powder does not increase on the contrary and reduces to some extent, the Containing Sulfur sodium of the low iron Sodium Sulphide of by-product is 60～72% simultaneously, and product reaches the technical indicator of GB GB/T 10500-2000.
3, the present invention simplifies the production technique of Strontium carbonate powder, and is simple to operate, flow process is short, equipment material is less demanding, and facility investment is little, and major and minor produce market demand is all vigorous, has good economic benefits.
Embodiment
Embodiment 1, be that 55～70% lazurite breeze mixes with the part by weight of reduction coal dust with 1: 1～1: 1.5 with Strontium Sulphate content, obtained grey black in 4～5 hours at 1100～1200 ℃ roasting temperatures, water counter-current extraction 3 times, obtain leaching liquid A, with soak slag a, use another part of leaching liquid A counter-current extraction grey black again, obtain leaching liquid B and soak slag b, leach the 3rd part of grey black once more with leaching liquid B and obtain leaching liquid C and soak slag c; Merge and soak slag a, b, c, stack for always soaking slag; Resulting leaching liquid C is that Sr content (in SrS) is the yellow water of 50～200g/L.
Get 3 liters of yellow waters that contain SrS 153g/L, place the batch reactor that has stirring, add 136g industrial solid soda ash soda ash reaction (solid soda ash adds continuously by feeding screw) again, temperature of reaction is 90 ℃, the reinforced time of soda ash is 20 minutes, and reaction 1.5 hours, centrifugation gained Strontium carbonate powder slip are continued in the reinforced back that finishes, solid is used 200mL water countercurrent washing 4 times respectively, dries down at 110 ℃ and obtains strontium carbonate product.Strontium carbonate product is a white powder, after measured, granularity D50=3.764 μ m, chemical analysis foreign matter content (massfraction) is respectively: CaCO
30.5%, BaCO
30.3%, Na 0.10%, Fe
2O
30.01%, Cl 0.08%, and S 0.06%, P
2O
50.01%, moisture 0.35%, hydrochloric acid insoluble substance 0.12%.
The mother liquor first time of washing Strontium carbonate powder is merged with the centrifuge mother liquor of Strontium carbonate powder slip,, obtain hanging down iron Sodium Sulphide byproduct by being the vacuum-evaporator evaporation of medium with the thermal oil.Low iron Sodium Sulphide is light orange, and chemical analysis results is: Na
2S 64%, Na
2SO
31.0%, Na
2S
2O
31.0%, TFe 0.0025%, Na
2CO
32.25%, water-insoluble 0.05%.
Embodiment 2, be that 55～70% lazurite breeze mixes with the part by weight of reduction coal dust with 1: 1～1: 1.5 with Strontium Sulphate content, obtained grey black in 4～5 hours at 1100～1200 ℃ roasting temperatures, water counter-current extraction 3 times, obtain leaching liquid A, with soak slag a, use another part of leaching liquid A counter-current extraction grey black again, obtain leaching liquid B and soak slag b, leach the 3rd part of grey black once more with leaching liquid B and obtain leaching liquid C and soak slag c; Merge and soak slag a, b, c, stack for always soaking slag; Resulting leaching liquid C is that Sr content (in SrS) is the yellow water of 50～200g/L.
Get the 3 liters of batch reactors that place stirring of yellow water that contain SrS 50g/L (0.4417mol/L), the 40% industrial liquid soda ash reaction (liquid soda ash adopts header tank to be metered into) that adds 492mL again, temperature of reaction is 90 ℃, the reinforced time of soda ash is 40 minutes, the reinforced back that finishes is continued reaction and is carried out solid-liquid separation after 0.5 hour, solid is used 100mL water countercurrent washing 4 times respectively, and under 110 ℃, dry strontium carbonate product.Strontium carbonate product is a white powder, after measured its granularity D
50=3.764 μ m, chemical analysis foreign matter content (massfraction) is respectively: CaCO
30.3%, BaCO
30.3%, Na 0.08%, Fe
2O
30.008%, Cl 0.05%, SO
40.15%, P
2O
50.01%, moisture 0.35%, hydrochloric acid insoluble substance 0.10%.
The mother liquor first time of washing Strontium carbonate powder is merged with the centrifuge mother liquor of Strontium carbonate powder slip,, obtain hanging down iron Sodium Sulphide byproduct by being the vacuum-evaporator evaporation of medium with the thermal oil.Low iron Sodium Sulphide is light orange, and chemical analysis results is: Na
2S 72%, Na
2SO
30.8%, Na
2S
2O
31.0%, TFe 0.0023%, Na
2CO
32.10%, water-insoluble 0.05%.
Claims (3)
1, a kind of is the method for raw material production high-quality strontium carbonate product with the celestite ore, comprises following processing step:
1. the lazurite breeze is mixed with the part by weight of reduction coal dust with 1: 0.5～1: 5, obtained grey black in 0.5～10 hour, again grey black water counter-current extraction is got strontium sulfide solution at 900～1300 ℃ roasting temperatures; Strontium sulfide solution concentration is controlled at 100～250g/L; Strontium Sulphate content is 55～75% in the described lazurite breeze;
2. the soda ash that adds strontium sulfide molar weight 95～105% under agitation in 90～100 ℃ of reactions 0.5～5 hour, generates and contains the Strontium carbonate powder precipitation and hang down the slip of iron Gas with Sodium Sulfide Solution;
3. slip is obtained the Strontium carbonate powder precipitation and hangs down the iron Gas with Sodium Sulfide Solution by centrifugation;
4. with Strontium carbonate powder water countercurrent washing 3～5 times, drying obtains the high-quality strontium carbonate product; The mother liquor first time of washing Strontium carbonate powder is merged with the low iron Gas with Sodium Sulfide Solution that 3. step obtains,, obtain hanging down iron Sodium Sulphide byproduct by being the vacuum-evaporator evaporation of medium with the thermal oil.
2, the production method of high-quality strontium carbonate product according to claim 1, it is characterized in that: the described raw coal of going back is coking coal, non-caking coal, lean coal, bottle coal, rich coal, any in long-flame coal, the hard coal.
3, the production method of high-quality strontium carbonate product according to claim 1, it is characterized in that: described soda ash is calcined soda for industry solution or solid soda ash.
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101559964B (en) * | 2009-05-19 | 2011-05-25 | 中国科学院青海盐湖研究所 | Preparation method of platy strontium carbonate particles |
| CN104192882B (en) * | 2014-08-15 | 2016-08-24 | 中国科学院过程工程研究所 | The method of Synthesis strontium carbonate is reduced-pressurizeed to a kind of celestite ore high temperature static |
| CN105776300A (en) * | 2016-01-29 | 2016-07-20 | 常州创索新材料科技有限公司 | Method for preparing high-purity strontium carbonate |
| CN106586975A (en) * | 2016-11-28 | 2017-04-26 | 江苏大学 | Process for reducing celestine in rotary hearth furnace to produce strontium sulfide |
| CN107601543B (en) * | 2017-10-28 | 2018-11-23 | 公碧燕 | Strontium carbonate and its production method |
| CN110589777A (en) * | 2019-09-27 | 2019-12-20 | 仝六斗 | Processing and extracting process for barite or celestite |
| CN115432728B (en) * | 2022-10-11 | 2023-04-28 | 南京工程学院 | Method for producing high-purity strontium carbonate by utilizing hydrogen metallurgy technology |
| CN115637336B (en) * | 2022-10-18 | 2024-01-30 | 中国地质科学院矿产综合利用研究所 | Process for preparing strontium carbonate from high barium strontium ore |
Citations (4)
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|---|---|---|---|---|
| CN1104608A (en) * | 1993-12-30 | 1995-07-05 | 梁义勋 | Production method of strontium carbonate |
| US6159436A (en) * | 1996-11-18 | 2000-12-12 | Centro De Investigacion Y De Estudios Avanzados Del I.P.N. | Conversion process for strontium sulfate in carbonate rich celestite ores to strontium carbonate using sodium carbonate in an air/vapor-lift loop reactor |
| CN1398788A (en) * | 2001-07-19 | 2003-02-26 | 冉天孝 | Regenerating circulation process of producing strontium carbonate |
| CN1699178A (en) * | 2005-05-11 | 2005-11-23 | 重庆大学 | Process for preparing high purity strontium carbonate |
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2007
- 2007-05-24 CN CN 200710018051 patent/CN100560500C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1104608A (en) * | 1993-12-30 | 1995-07-05 | 梁义勋 | Production method of strontium carbonate |
| US6159436A (en) * | 1996-11-18 | 2000-12-12 | Centro De Investigacion Y De Estudios Avanzados Del I.P.N. | Conversion process for strontium sulfate in carbonate rich celestite ores to strontium carbonate using sodium carbonate in an air/vapor-lift loop reactor |
| CN1398788A (en) * | 2001-07-19 | 2003-02-26 | 冉天孝 | Regenerating circulation process of producing strontium carbonate |
| CN1699178A (en) * | 2005-05-11 | 2005-11-23 | 重庆大学 | Process for preparing high purity strontium carbonate |
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