CN102153122A - Method for reducing sulphur content of strontium carbonate product - Google Patents
Method for reducing sulphur content of strontium carbonate product Download PDFInfo
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- CN102153122A CN102153122A CN 201110096382 CN201110096382A CN102153122A CN 102153122 A CN102153122 A CN 102153122A CN 201110096382 CN201110096382 CN 201110096382 CN 201110096382 A CN201110096382 A CN 201110096382A CN 102153122 A CN102153122 A CN 102153122A
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- strontium carbonate
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Abstract
The invention relates to a method for reducing sulphur content of a strontium carbonate product. The method includes the steps as follows: (1) mixing strontium carbonate power with water according to a solid-liquid mass ratio of 1:6-10 and stirring the mixture to form uniform slurry; (2) at the stirring state, adding a desulphurizing agent in the slurry, raising temperature to 90-105 DEG C and keeping the temperature for 30-120min, and obtaining desulphurized slurry; and (3) separating the desulphurized slurry to obtain mother liquor and a filter cake, precipitating or settling the mother liquor by lime milk to obtain thiosulfate precipitate of calcium and pure water, wherein the pure water returns to the production stage of strontium carbonate, and the thiosulfate precipitate of the calcium is stacked as waste residue; and washing and drying the filter cake to obtain desulphurized strontium carbonate product. The method can effectively reduce consumption during treatment processes, avoid pollution, convert solid free sulphur to dissolvable thiosulfate, not only lower the content of the free sulphur in the product, but also improve the quality and the additional value of the strontium carbonate product.
Description
Technical field
The present invention relates to the Strontium carbonate powder production field, relate in particular to a kind of method that reduces strontium carbonate product free sulphur content.
Background technology
Strontium carbonate powder is mainly used in fields such as electronics, magneticsubstance, fluorescent material and war products, and Strontium carbonate powder content in the product powder and total sulfur foreign matter content are most important to exploitation and the suitability of using the field.
The technology that with the celestite ore is the raw material production Strontium carbonate powder mainly contains metathesis conversion method and carbon reduction method.
The metathesis conversion method is that the reaction of lazurite breeze and volatile salt is generated thick Strontium carbonate powder, and thick Strontium carbonate powder is through acid (or ammonium salt) dissolving, refiningly obtains more purified accordingly strontium salt solution, recyclable volatile salt during the ammonium salt dissolving after removing impurity such as calcium, barium; The volatile salt carbonization that adds after making with extra care in the strontium salt solution obtains strontium carbonate product and ammonium salt dilute solution.The utilization ratio that this method advantage is lazurite is higher, good quality of product, the subject matter that exists is required ore grade height, thick Strontium carbonate powder acid a large amount of hydrochloric acid of molten treating process consumption or ammonium salt and a large amount of industrial chemicals, particularly adopt the ammonium salt dissolving, the slip of carbonization separates filter cake washing can produce a large amount of ammonium salt dilute solutions, and cyclic utilization rate is low; In addition, ammonium salt-containing discharge of wastewater serious environment pollution is subjected to the restriction of environmental requirement.Show according to pertinent data, adopt the production equipment of this technology at present in the world
Close All.
Carbon reduction method is after coal dust mixes with reduction with the lazurite breeze, at 1100～1150 ℃ of strontium sulfide grogs that are reduced into solubility, the hot water leaching, obtains strontium sulfide solution, employing CO after separating waste residue
2Carbonization obtains strontium carbonate product and by product H
2S gas, H
2S is used to produce sulphur or thiocarbamide after reclaiming, and this is present domestic and international topmost production method.This processing unit is simple, easy to operate, and subject matter one is that environmental pollution is serious, sulfur-bearing " three wastes " difficult treatment, and exist potential safety hazards such as hydrogen sulfide leakage; The 2nd, sulphur content is higher in the product, can't satisfy the specification of quality of users at home and abroad to high-quality strontium carbonate.
Generally, the strontium carbonate product of above-mentioned two kinds of explained hereafter can satisfy general industrial use substantially, but carbon reduction technology is in reducing roasting, leaching and carbonic acid gas carbonization gas preparation process, be subjected to factor affecting such as air pressure, oxygen content and temperature, carbonization process very easily produces free sulphur, and be dispersed in the split with trickle state, limited the application of product in fields such as electronic material, alloy preparations.
China is the abundantest country of lazurite resource reserve in the world, mainly be distributed in ground such as the Caidamu Basin, Qinghai, Huangshi, Chongqing and Lishui, Jiangsu, constantly enlarge along with exploiting scale for many years, ore reserves is quick downtrending, and the resource exhaustion phenomenon has appearred in indivedual areas.Area, Qaidam, Qinghai is because of condition influence such as industrial development levels, still be in the primary stage of lazurite development of resources, though the raw ore grade is lower, but reserves account for the whole nation nearly 70%, extensive ore-dressing plant and Strontium carbonate powder production equipment have been built up, along with the quickening of western development of resources paces, will progressively develop into most important in the world strontium products production base.As previously mentioned, be subjected to factor affecting such as weather, sulphur content is higher in the strontium carbonate product, has restricted the product performance of competitive edge on the market at home and abroad, has influenced the Sustainable development of regional strontium industry.
Summary of the invention
Technical problem to be solved by this invention provide a kind of effective reduction treating processes consumption, avoid producing the method for the reduction strontium carbonate product sulphur content of pollution.
For addressing the above problem, a kind of method that reduces the strontium carbonate product sulphur content of the present invention may further comprise the steps:
(1) dried strontium carbonate powder is mixed with water by 1: 6～10 solid-liquid mass ratio, and stir into distributed slurry;
(2) in described slip, add sulfur elimination, under whipped state, be warming up to 90～105 ℃, and under this temperature, be incubated 30～120min, obtain falling the slip behind the sulphur;
(3) fall slip behind the sulphur after separating with described, obtain mother liquor and filter cake; Described mother liquor obtains the thiosulphate precipitation and the water purification of calcium after milk of lime precipitation or sedimentation processing, water purification returns Strontium carbonate powder production workshop section, and the thiosulphate of calcium is stacked as waste residue; Described filter cake is through washing, after the drying, obtains falling the strontium carbonate product behind the sulphur.
Strontium carbonate powder in the described step (1) is meant the strontium carbonate product that the lazurite breeze is produced through carbon reduction-water extraction-carbonic acid gas carbonization technique.
Sulfur elimination in the described step (2) is meant that mass concentration in the slip system is that 0.2～0.5% S-WAT and mass concentration are that 0.2～1.0% sodium hydroxide or mass concentration are the combination of 0.5～1.6% yellow soda ash.
The present invention compared with prior art has the following advantages:
1, the way that the present invention utilizes chemical agent to handle, adopt the higher strontium carbonate product of free sulphur content that causes because of factors such as barometric point and oxygen contents of pyrocarbon reduction-water extraction-carbonic acid gas carbonization technique production to handle to Qaidam, Qinghai area, make that solid-state free sulphur is converted into the solubility thiosulphate in the strontium carbonate product, not only fully reduced free sulphur content in the product, and strontium carbonate product quality and added value have been improved, reach the requirement of world market, thereby can be widely used in the needs that the downstream high-end product is produced the high-quality strontium carbonate product.
2, because desulfurization of the present invention processing dosing is few, therefore, reduced production cost effectively.
3, because after the slip separation after handling among the present invention, therefore the equal recycle of mother liquor and washing lotion, not only effectively reduces the consumption in the treating processes, and does not produce " three wastes " pollutent.
4, treating process of the present invention and equipment are simple, are easy to operate and control, and also can directly dock with the Strontium carbonate powder production equipment, and is practical.
Embodiment
1 one kinds of methods that reduce the strontium carbonate product sulphur content of embodiment may further comprise the steps:
(1) (dry back total sulfur content counts 0.6165% with S, and the national Specification total sulfur content is no more than 0.15% with dried strontium carbonate powder.) mixing in the stock tank again with water by 1: 6 solid-liquid mass ratio (kg/kg), and stir into distributed slurry.
(2) in slip, add sulfur elimination---make slip system Central Asia sodium sulfate, sodium hydroxide mass concentration be respectively 0.2%, continue stirring and dissolving, pump into closed reactor then, under whipped state, be warming up to 90 ℃, the solid phase free sulphur in the Strontium carbonate powder is transformed to soluble salt.Under this temperature, be incubated 30min then, make the solid phase free sulphur be converted into soluble salt and be dissolved in the liquid phase, finally obtain falling the slip behind the sulphur.
(3) slip behind the sulphur be will fall after closed whizzer separates with the speed of 1200r/min, mother liquor and filter cake obtained.
Mother liquor obtains the thiosulphate precipitation and the upper strata water purification of throw out calcium after milk of lime precipitation or sedimentation processing, this water purification returns Strontium carbonate powder production workshop section, is used for the leaching of process for producing strontium carbonate grey black, and the thiosulphate of calcium is stacked as waste residue.
Filter cake adopts the mode (spraying with tap water in whizzer) of spray to wash, and detects through chemical qualitativity until filtrate, does not contain till the water-soluble S-contained substance existence; Then with filter cake after drying under 110～115 ℃ of temperature, obtain falling the strontium carbonate product behind the sulphur.Washing lotion then is used for the batching water that step (1) desulfurization is handled.Press Strontium carbonate powder GB analytical test behind the filtration cakes torrefaction, total sulfur content 0.1513% in the product, sulfur removal effectiveness 75.46%.The product total sulfur content meets the GB regulation.
2 one kinds of methods that reduce the strontium carbonate product sulphur content of embodiment may further comprise the steps:
(1) (dry back total sulfur content counts 0.6165% with S, and the national Specification total sulfur content is no more than 0.15% with dried strontium carbonate powder.) mixing in the stock tank again with water by 1: 10 solid-liquid mass ratio (kg/kg), and stir into distributed slurry.
(2) in slip, add sulfur elimination---make slip system Central Asia sodium sulfate, sodium hydroxide mass concentration be respectively 0.5% and 1.0%, continue stirring and dissolving, pump into closed reactor then, under whipped state, be warming up to 105 ℃, the solid phase free sulphur in the Strontium carbonate powder is transformed to soluble salt.Under this temperature, be incubated 120min then, make the solid phase free sulphur be converted into soluble salt and be dissolved in the liquid phase.
(3) slip behind the sulphur be will fall after closed whizzer separates with the speed of 1200r/min, mother liquor and filter cake obtained.
Mother liquor obtains the thiosulphate precipitation and the upper strata water purification of throw out calcium after milk of lime precipitation or sedimentation processing, this water purification returns Strontium carbonate powder production workshop section, is used for the leaching of process for producing strontium carbonate grey black, and the thiosulphate of calcium is stacked as waste residue.
Filter cake adopts the mode (spraying with tap water in whizzer) of spray to wash, and detects through chemical qualitativity until filtrate, does not contain till the water-soluble S-contained substance existence; Then with filter cake after drying under 110～115 ℃ of temperature, obtain falling the strontium carbonate product behind the sulphur.Washing lotion then is used for the batching water that step (1) desulfurization is handled.Press Strontium carbonate powder GB analytical test behind the filtration cakes torrefaction, total sulfur content 0.1439% in the product, sulfur removal effectiveness 76.66%.The product total sulfur content meets the GB regulation.
3 one kinds of methods that reduce the strontium carbonate product sulphur content of embodiment may further comprise the steps:
(1) (dry back total sulfur content counts 0.6165% with S, and the national Specification total sulfur content is no more than 0.15% with dried strontium carbonate powder.) mixing in the stock tank again with water by 1: 7 solid-liquid mass ratio (kg/kg), and stir into distributed slurry.
(2) in slip, add sulfur elimination---make slip system Central Asia sodium sulfate, sodium hydroxide mass concentration be respectively 0.3% and 0.5%, continue stirring and dissolving, pump into closed reactor then, under whipped state, be warming up to 100 ℃, the solid phase free sulphur in the Strontium carbonate powder is transformed to soluble salt.Under this temperature, be incubated 60min then, make the solid phase free sulphur be converted into soluble salt and be dissolved in the liquid phase.
(3) slip behind the sulphur be will fall after closed whizzer separates with the speed of 1200r/min, mother liquor and filter cake obtained.
Mother liquor obtains the thiosulphate precipitation and the upper strata water purification of throw out calcium after milk of lime precipitation or sedimentation processing, this water purification returns Strontium carbonate powder production workshop section, is used for the leaching of process for producing strontium carbonate grey black, and the thiosulphate of calcium is stacked as waste residue.
Filter cake adopts the mode (spraying with tap water in whizzer) of spray to wash, and detects through chemical qualitativity until filtrate, does not contain till the water-soluble S-contained substance existence; Then with filter cake after drying under 110～115 ℃ of temperature, obtain falling the strontium carbonate product behind the sulphur.Washing lotion then is used for the batching water that step (1) desulfurization is handled.Press Strontium carbonate powder GB analytical test behind the filtration cakes torrefaction, total sulfur content 0.1526% in the product, sulfur removal effectiveness 75.25%.The product total sulfur content meets the GB regulation.
4 one kinds of methods that reduce the strontium carbonate product sulphur content of embodiment may further comprise the steps:
(1) (dry back total sulfur content counts 0.6165% with S, and the national Specification total sulfur content is no more than 0.15% with dried strontium carbonate powder.) mixing in the stock tank again with water by 1: 6 solid-liquid mass ratio (kg/kg), and stir into distributed slurry.
(2) in slip, adding sulfur elimination---the mass concentration that makes slip system Central Asia sodium sulfate is 0.2%, the mass concentration of yellow soda ash is 0.5%, continue stirring and dissolving, pump into closed reactor then, under whipped state, be warming up to 90 ℃, the solid phase free sulphur in the Strontium carbonate powder is transformed to soluble salt.Under this temperature, be incubated 30min then, make the solid phase free sulphur be converted into soluble salt and be dissolved in the liquid phase.
(3) slip behind the sulphur be will fall after closed whizzer separates with the speed of 1200r/min, mother liquor and filter cake obtained.
Mother liquor obtains the thiosulphate precipitation and the upper strata water purification of throw out calcium after milk of lime precipitation or sedimentation processing, this water purification returns Strontium carbonate powder production workshop section, is used for the leaching of process for producing strontium carbonate grey black, and the thiosulphate of calcium is stacked as waste residue.
Filter cake adopts the mode (spraying with tap water in whizzer) of spray to wash, and detects through chemical qualitativity until filtrate, does not contain till the water-soluble S-contained substance existence; Then with filter cake after drying under 110～115 ℃ of temperature, obtain falling the strontium carbonate product behind the sulphur.Washing lotion then is used for the batching water that step (1) desulfurization is handled.Press Strontium carbonate powder GB analytical test behind the filtration cakes torrefaction, total sulfur content 0.1522% in the product, sulfur removal effectiveness 75.31%.The product total sulfur content meets the GB regulation.
5 one kinds of methods that reduce the strontium carbonate product sulphur content of embodiment may further comprise the steps:
(1) (dry back total sulfur content counts 0.6165% with S, and the national Specification total sulfur content is no more than 0.15% with dried strontium carbonate powder.) mixing in the stock tank again with water by 1: 10 solid-liquid mass ratio (kg/kg), and stir into distributed slurry.
(2) in slip, adding sulfur elimination---the mass concentration that makes slip system Central Asia sodium sulfate is 0.5%, the mass concentration of yellow soda ash is 1.6%, continue stirring and dissolving, pump into closed reactor then, under whipped state, be warming up to 105 ℃, the solid phase free sulphur in the Strontium carbonate powder is transformed to soluble salt.Under this temperature, be incubated 120min then, make the solid phase free sulphur be converted into soluble salt and be dissolved in the liquid phase.
(3) slip behind the sulphur be will fall after closed whizzer separates with the speed of 1200r/min, mother liquor and filter cake obtained.
Mother liquor obtains the thiosulphate precipitation and the upper strata water purification of throw out calcium after milk of lime precipitation or sedimentation processing, this water purification returns Strontium carbonate powder production workshop section, is used for the leaching of process for producing strontium carbonate grey black, and the thiosulphate of calcium is stacked as waste residue.
Filter cake adopts the mode (spraying with tap water in whizzer) of spray to wash, and detects through chemical qualitativity until filtrate, does not contain till the water-soluble S-contained substance existence; Then with filter cake after drying under 110～115 ℃ of temperature, obtain falling the strontium carbonate product behind the sulphur.Washing lotion then is used for the batching water that step (1) desulfurization is handled.Press Strontium carbonate powder GB analytical test behind the filtration cakes torrefaction, total sulfur content 0.1443% in the product, sulfur removal effectiveness 76.59%.The product total sulfur content meets the GB regulation.
6 one kinds of methods that reduce the strontium carbonate product sulphur content of embodiment may further comprise the steps:
(1) (dry back total sulfur content counts 0.6165% with S, and the national Specification total sulfur content is no more than 0.15% with dried strontium carbonate powder.) mixing in the stock tank again with water by 1: 6 solid-liquid mass ratio (kg/kg), and stir into distributed slurry.
(2) in slip, adding sulfur elimination---the mass concentration that makes slip system Central Asia sodium sulfate is 0.3%, the mass concentration of yellow soda ash is 1.0%, continue stirring and dissolving, pump into closed reactor then, under whipped state, be warming up to 100 ℃, the solid phase free sulphur in the Strontium carbonate powder is transformed to soluble salt.Under this temperature, be incubated 60min then, make the solid phase free sulphur be converted into soluble salt and be dissolved in the liquid phase.
(3) slip behind the sulphur be will fall after closed whizzer separates with the speed of 1200r/min, mother liquor and filter cake obtained.
Mother liquor obtains the thiosulphate precipitation and the upper strata water purification of throw out calcium after milk of lime precipitation or sedimentation processing, this water purification returns Strontium carbonate powder production workshop section, is used for the leaching of process for producing strontium carbonate grey black, and the thiosulphate of calcium is stacked as waste residue.
Filter cake adopts the mode (spraying with tap water in whizzer) of spray to wash, and detects through chemical qualitativity until filtrate, does not contain till the water-soluble S-contained substance existence; Then with filter cake after drying under 110～115 ℃ of temperature, obtain falling the strontium carbonate product behind the sulphur.Washing lotion then is used for the batching water that step (1) desulfurization is handled.Press Strontium carbonate powder GB analytical test behind the filtration cakes torrefaction, total sulfur content 0.1540% in the product, sulfur removal effectiveness 75.02%.The product total sulfur content meets the GB regulation.
Strontium carbonate powder in the foregoing description 1～6 step (1) is meant the strontium carbonate product that the lazurite breeze is produced through carbon reduction-water extraction-carbonic acid gas carbonization technique.
Claims (3)
1. method that reduces the strontium carbonate product sulphur content may further comprise the steps:
(1) dried strontium carbonate powder is mixed with water by 1: 6～10 solid-liquid mass ratio, and stir into distributed slurry;
(2) in described slip, add sulfur elimination, under whipped state, be warming up to 90～105 ℃, and under this temperature, be incubated 30～120min, obtain falling the slip behind the sulphur;
(3) fall slip behind the sulphur after separating with described, obtain mother liquor and filter cake; Described mother liquor obtains the thiosulphate precipitation and the water purification of calcium after milk of lime precipitation or sedimentation processing, water purification returns Strontium carbonate powder production workshop section, and the thiosulphate of calcium is stacked as waste residue; Described filter cake is through washing, after the drying, obtains falling the strontium carbonate product behind the sulphur.
2. a kind of method that reduces the strontium carbonate product sulphur content as claimed in claim 1 is characterized in that: the strontium carbonate powder in the described step (1) is meant the strontium carbonate product that the lazurite breeze is produced through carbon reduction-water extraction-carbonic acid gas carbonization technique.
3. a kind of method that reduces the strontium carbonate product sulphur content as claimed in claim 1 is characterized in that: the sulfur elimination in the described step (2) is meant that mass concentration in the slip system is that 0.2～0.5% S-WAT and mass concentration are that 0.2～1.0% sodium hydroxide or mass concentration are the combination of 0.5～1.6% yellow soda ash.
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| CN 201110096382 CN102153122A (en) | 2011-04-13 | 2011-04-13 | Method for reducing sulphur content of strontium carbonate product |
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| CN 201110096382 CN102153122A (en) | 2011-04-13 | 2011-04-13 | Method for reducing sulphur content of strontium carbonate product |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104307349A (en) * | 2014-10-24 | 2015-01-28 | 重庆庆龙精细锶盐化工有限公司 | Washable serial type strontium slurry desulfurization system |
| CN104324601A (en) * | 2014-10-24 | 2015-02-04 | 重庆庆龙精细锶盐化工有限公司 | Energy-saving strontium pulp desulfurization system |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1059319A (en) * | 1991-07-15 | 1992-03-11 | 重庆五兴复合材料化工研究所 | Strontium carbonate powder-smart S-WAT joint process |
-
2011
- 2011-04-13 CN CN 201110096382 patent/CN102153122A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1059319A (en) * | 1991-07-15 | 1992-03-11 | 重庆五兴复合材料化工研究所 | Strontium carbonate powder-smart S-WAT joint process |
Non-Patent Citations (2)
| Title |
|---|
| 《IM&P 化工矿物与加工》 20101031 郭金禹等 碳酸锶产品降硫工艺技术研究 21-23 1-3 , 第10期 * |
| 《辽宁化工》 20030209 邸万山等 硫代硫酸钠合成条件的优化 54-55 3 第32卷, 第2期 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104307349A (en) * | 2014-10-24 | 2015-01-28 | 重庆庆龙精细锶盐化工有限公司 | Washable serial type strontium slurry desulfurization system |
| CN104324601A (en) * | 2014-10-24 | 2015-02-04 | 重庆庆龙精细锶盐化工有限公司 | Energy-saving strontium pulp desulfurization system |
| CN104324601B (en) * | 2014-10-24 | 2023-07-25 | 重庆庆龙精细锶盐化工有限公司 | Energy-saving strontium slurry desulfurization system |
| CN104307349B (en) * | 2014-10-24 | 2023-07-25 | 重庆庆龙精细锶盐化工有限公司 | Flushable serial strontium slurry desulfurization system |
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Application publication date: 20110817 |