CN102617054B - Method for preparing dolomite magnesia from bischofite and dolomite - Google Patents
Method for preparing dolomite magnesia from bischofite and dolomite Download PDFInfo
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- CN102617054B CN102617054B CN201210066762.2A CN201210066762A CN102617054B CN 102617054 B CN102617054 B CN 102617054B CN 201210066762 A CN201210066762 A CN 201210066762A CN 102617054 B CN102617054 B CN 102617054B
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- dolomite
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Abstract
The invention relates to a method for preparing dolomite magnesia from bischofite and dolomite. The method comprises the following steps of: firstly, grinding calcined dolomite into dolomite powder and digesting the dolomite powder into caustic dolomite lime milk by using a calcium chloride solution; secondly, preparing a magnesium chloride solution; thirdly, carrying out stirring reaction on the magnesium chloride solution and the caustic dolomite lime milk in a constant-temperature water bath to generate magnesium hydroxide precipitation; fourthly, washing the magnesium hydroxide precipitation with water and carrying out suction filtration to obtain a filter cake and a primary washing water and mother solution merged substance; fifthly, reacting the primary washing water and mother solution merged substance with the caustic dolomite lime milk to generate a calcium-magnesium hydroxide sediment; sixthly, filtering and washing the calcium-magnesium hydroxide sediment and lightly burning the washed sediment to obtain a primary raw material of the dolomite magnesia; and seventhly, pressing the primary raw material to form a brick body with 300*150mm*100mm and carrying out dead burning in a high-temperature kiln to obtain the dolomite magnesia. The method disclosed by the invention has the advantages of simple process, high quality of products, low cost and easiness in realization of industrial production.
Description
Technical field
The present invention relates to a kind of preparation method of magnesium compound, relate in particular to a kind of by bischofite and dolomite made the method for rhombspar magnesia.
Background technology
Magnesia is the basic refractory of a kind of high purity, high-melting-point, compact structure, is widely used in the numerous areas such as smelting iron and steel, glass industry, Cement industry, family's electric heater and pyrochemistry industry.China is that magnesia is produced and big export country in the world.At present, produce the shortcomings such as the method for magnesia is normally formed by the magnesium oxide high-temperature calcination of wagnerite and the extraction of seawater (or bittern) magnesite, and the method exists complex process, energy consumption is high, waste liquid amount is large, big for environment pollution, product purity is low.
Summary of the invention
Technical problem to be solved by this invention is to provide that a kind of technique is simple, good product quality, with low cost by bischofite and dolomite made the method for rhombspar magnesia.
For addressing the above problem, of the present invention a kind of by bischofite and dolomite made for the method for rhombspar magnesia, comprise the following steps:
(1) the rhombspar of 900 ℃ ~ 1000 ℃ of calcinings is ground to form to 180 object rhombspar powder, this rhombspar powder is digested to caustic dolomite ash breast with the calcium chloride solution of 3 ~ 8 times of its quality; In described calcium chloride solution, calcium chloride mass content is 1% ~ 20%;
(2) prepare magnesium chloride solution: it is 1.19 ~ 1.23g/cm that bischofite water is dissolved into proportion
3magnesium chloride solution;
(3) the stirring reaction in 20 ℃ ~ 60 ℃ waters bath with thermostatic control by described magnesium chloride solution and described caustic dolomite ash breast, generated magnesium hydrate precipitate after 5 ~ 30 minutes; The mass ratio of wherein said magnesium chloride solution and described calcium chloride solution is 1:0.5 ~ 1;
(4) described magnesium hydrate precipitate is washed with the water of its 0.3 ~ 0.5 times of quality, then carry out suction filtration, obtain filter cake and wash water and this mother liquor of mother liquor A(and refer to the liquid that suction filtration directly obtains); Described filter cake is dried to constant weight and after 500 ~ 600 ℃ of temperature lower calcinations, is obtained magnesium cement magnesium oxide; A described wash water and mother liquor A consolidated material be the raw material for magnesia as the supply system;
By described step wash water in (4) and mother liquor A consolidated material again with described step (1) in the caustic dolomite ash breast of gained with the mass ratio of 1:1, react generation calcium-magnesium precipitation of hydroxide thing;
(6) by described step calcium-magnesium precipitation of hydroxide thing (5) after filtration, after washing, at 700 ~ 800 ℃ of light-burned one-tenth rhombspar magnesia primary raw materialss, and obtain wash water and this mother liquor of mother liquor B(refers to the liquid that suction filtration directly obtains); Described wash water is sent to digestion caustic dolomite, and described mother liquor B sends to processing water resistant additive or calcium chloride;
By described step primary raw materials (6) under 100MPa ~ 200MPa pressure, be pressed into the brick body of 300 * 150 * 100mm, then dead roasting in the high temperature kiln of 1500 ~ 1600 ℃, obtains rhombspar magnesia.
The described step (1) temperature of middle digestion reaction is 30 ℃ ~ 40 ℃.
Described step (3) middle stirring velocity is 100 ~ 200 revs/min.
Described step (4) middle mode of washing is countercurrent washing.
The present invention compared with prior art has the following advantages:
1, the present invention takes full advantage of China western abundant magnesium chloride and dolomite resources, and therefore, it is easy, convenient that raw material obtains, and cheap.
2, simple, the environmentally safe of production technique of the present invention, and equipment requirements is low, is easy to realize suitability for industrialized production; The all technical of gained rhombspar magnesia all can reach the standard of magnesia.
Embodiment
embodiment 1by bischofite and dolomite made, for a method for rhombspar magnesia, comprised the following steps:
(1) the rhombspar of 900 ℃ of calcinings is ground to form to 180 object rhombspar powder; Get 100 grams of these rhombspar powder and put into beaker, and 600 grams of calcium chloride solutions are joined in the above-mentioned beaker that fills rhombspar powder, at 30 ℃ ~ 40 ℃ temperature, be digested to caustic dolomite ash breast.
Wherein: in calcium chloride solution, calcium chloride mass content is 1%.
(2) prepare magnesium chloride solution: it is 1.19g/cm that bischofite water is dissolved into proportion
3magnesium chloride solution.
(3) 600 grams of magnesium chloride solutions being joined in the newborn beaker of above-mentioned caustic dolomite ash, and this beaker is placed in to HH-S6 type thermostat water bath, is that 30 ℃, rotating speed are stirring reaction under the condition of 100 revs/min at bath temperature, after 10 minutes, generates magnesium hydrate precipitate.
(4) magnesium hydrate precipitate is carried out to countercurrent washing with the water of its 0.3 times of quality, then carry out suction filtration, obtain filter cake and wash water and mother liquor A; Filter cake is dried to constant weight and after 500 ~ 600 ℃ of temperature lower calcinations, is obtained magnesium cement magnesium oxide; Wash water and mother liquor A consolidated material be the raw material for magnesia as the supply system.
By step wash water in (4) and mother liquor A consolidated material again with step (1) in the caustic dolomite ash breast of gained with the mass ratio of 1:1, react generation calcium-magnesium precipitation of hydroxide thing.
By step calcium-magnesium precipitation of hydroxide thing (5) after filtration, washing after, at 700 ℃ of light-burned one-tenth rhombspar magnesia primary raw materialss, and obtain wash water and mother liquor B; Wash water is sent to digestion caustic dolomite, and mother liquor B sends to processing water resistant additive or calcium chloride.
By step primary raw materials (6) under 100MPa pressure, be pressed into the brick body of 300 * 150 * 100mm, then dead roasting in the high temperature kiln of 1500 ℃, obtains rhombspar magnesia.
embodiment 2by bischofite and dolomite made, for a method for rhombspar magnesia, comprised the following steps:
(1) the rhombspar of 950 ℃ of calcinings is ground to form to 180 object rhombspar powder; Get 100 grams of these rhombspar powder and put into beaker, and 540 grams of calcium chloride solutions are joined in the above-mentioned beaker that fills rhombspar powder, at 30 ℃ ~ 40 ℃ temperature, be digested to caustic dolomite ash breast.
Wherein: in calcium chloride solution, calcium chloride mass content is 4%.
(2) prepare magnesium chloride solution: it is 1.20g/cm that bischofite water is dissolved into proportion
3magnesium chloride solution.
(3) 600 grams of magnesium chloride solutions being joined in the newborn beaker of above-mentioned caustic dolomite ash, and this beaker is placed in to HH-S6 type thermostat water bath, is that 35 ℃, rotating speed are stirring reaction under the condition of 150 revs/min at bath temperature, after 10 minutes, generates magnesium hydrate precipitate.
(4) magnesium hydrate precipitate is carried out to countercurrent washing with the water of its 0.4 times of quality, then carry out suction filtration, obtain filter cake and wash water and mother liquor A; Filter cake is dried to constant weight and after 500 ~ 600 ℃ of temperature lower calcinations, is obtained magnesium cement magnesium oxide; Wash water and mother liquor A consolidated material be the raw material for magnesia as the supply system.
By step wash water in (4) and mother liquor A consolidated material again with step (1) in the caustic dolomite ash breast of gained with the mass ratio of 1:1, react generation calcium-magnesium precipitation of hydroxide thing.
By step calcium-magnesium precipitation of hydroxide thing (5) after filtration, washing after, at 750 ℃ of light-burned one-tenth rhombspar magnesia primary raw materialss, and obtain wash water and mother liquor B; Wash water is sent to digestion caustic dolomite, and mother liquor B sends to processing water resistant additive or calcium chloride.
By step primary raw materials (6) under 120MPa pressure, be pressed into the brick body of 300 * 150 * 100mm, then dead roasting in the high temperature kiln of 1500 ℃, obtains rhombspar magnesia.
embodiment 3by bischofite and dolomite made, for a method for rhombspar magnesia, comprised the following steps:
(1) the rhombspar of 1000 ℃ of calcinings is ground to form to 180 object rhombspar powder; Get 100 grams of these rhombspar powder and put into beaker, and 450 grams of calcium chloride solutions are joined in the above-mentioned beaker that fills rhombspar powder, at 30 ℃ ~ 40 ℃ temperature, be digested to caustic dolomite ash breast.
Wherein: in calcium chloride solution, calcium chloride mass content is 5%.
(2) prepare magnesium chloride solution: it is 1.22g/cm that bischofite water is dissolved into proportion
3magnesium chloride solution.
(3) 600 grams of magnesium chloride solutions are joined in the newborn beaker of above-mentioned caustic dolomite ash,, and this beaker is placed in to HH-S6 type thermostat water bath, at bath temperature, be that 40 ℃, rotating speed are stirring reaction under the condition of 180 revs/min, after 8 minutes, generate magnesium hydrate precipitate.
(4) magnesium hydrate precipitate is carried out to countercurrent washing with the water of its 0.4 times of quality, then carry out suction filtration, obtain filter cake and wash water and mother liquor A; Filter cake is dried to constant weight and after 500 ~ 600 ℃ of temperature lower calcinations, is obtained magnesium cement magnesium oxide; Wash water and mother liquor A consolidated material be the raw material for magnesia as the supply system.
By step wash water in (4) and mother liquor A consolidated material again with step (1) in the caustic dolomite ash breast of gained with the mass ratio of 1:1, react generation calcium-magnesium precipitation of hydroxide thing.
By step calcium-magnesium precipitation of hydroxide thing (5) after filtration, washing after, at 750 ℃ of light-burned one-tenth rhombspar magnesia primary raw materialss, and obtain wash water and mother liquor B; Wash water is sent to digestion caustic dolomite, and mother liquor B sends to processing water resistant additive or calcium chloride.
By step primary raw materials (6) under 150MPa pressure, be pressed into the brick body of 300 * 150 * 100mm, then dead roasting in the high temperature kiln of 1500 ℃, obtains rhombspar magnesia.
embodiment 4by bischofite and dolomite made, for a method for rhombspar magnesia, comprised the following steps:
(1) the rhombspar of 1000 ℃ of calcinings is ground to form to 180 object rhombspar powder; Get 100 grams of these rhombspar powder and put into beaker, and 480 grams of calcium chloride solutions are joined in the above-mentioned beaker that fills rhombspar powder, at 30 ℃ ~ 40 ℃ temperature, be digested to caustic dolomite ash breast.
Wherein: in calcium chloride solution, calcium chloride mass content is 6%.
(2) prepare magnesium chloride solution: it is 1.23g/cm that bischofite water is dissolved into proportion
3magnesium chloride solution.
(3) 600 grams of magnesium chloride solutions being joined in the newborn beaker of above-mentioned caustic dolomite ash, and this beaker is placed in to HH-S6 type thermostat water bath, is stirring reaction under the condition of 200 revs/min of 40 ℃, rotating speed at bath temperature, after 6 minutes, generates magnesium hydrate precipitate.
(4) magnesium hydrate precipitate is carried out to countercurrent washing with the water of its 0.5 times of quality, then carry out suction filtration, obtain filter cake and wash water and mother liquor A; Filter cake is dried to constant weight and after 500 ~ 600 ℃ of temperature lower calcinations, is obtained magnesium cement magnesium oxide; Wash water and mother liquor A consolidated material be the raw material for magnesia as the supply system.
By step wash water in (4) and mother liquor A consolidated material again with step (1) in the caustic dolomite ash breast of gained with the mass ratio of 1:1, react generation calcium-magnesium precipitation of hydroxide thing.
By step calcium-magnesium precipitation of hydroxide thing (5) after filtration, washing after, at 800 ℃ of light-burned one-tenth rhombspar magnesia primary raw materialss, and obtain wash water and mother liquor B; Wash water is sent to digestion caustic dolomite, and mother liquor B sends to processing water resistant additive or calcium chloride.
By step primary raw materials (6) under 160MPa pressure, be pressed into the brick body of 300 * 150 * 100mm, then dead roasting in the high temperature kiln of 1550 ℃, obtains rhombspar magnesia.
embodiment 5by bischofite and dolomite made, for a method for rhombspar magnesia, comprised the following steps:
(1) the rhombspar of 1000 ℃ of calcinings is ground to form to 180 object rhombspar powder; Get 100 grams of these rhombspar powder and put into beaker, and 300 grams of calcium chloride solutions are joined and in the above-mentioned beaker that fills rhombspar powder, at 30 ℃ ~ 40 ℃ temperature, are digested to caustic dolomite ash breast.
Wherein: in calcium chloride solution, calcium chloride mass content is 6%.
(2) prepare magnesium chloride solution: it is 1.23g/cm that bischofite water is dissolved into proportion
3magnesium chloride solution.
(3) 600 grams of magnesium chloride solutions being joined in the newborn beaker of above-mentioned caustic dolomite ash, and this beaker is placed in to HH-S6 type thermostat water bath, is stirring reaction under the condition of 200 revs/min of 40 ℃, rotating speed at bath temperature, after 6 minutes, generates magnesium hydrate precipitate.
(4) magnesium hydrate precipitate is carried out to countercurrent washing with the water of its 0.5 times of quality, then carry out suction filtration, obtain filter cake and wash water and mother liquor A; Filter cake is dried to constant weight and after 500 ~ 600 ℃ of temperature lower calcinations, is obtained magnesium cement magnesium oxide; Wash water and mother liquor A consolidated material be the raw material for magnesia as the supply system.
By step wash water in (4) and mother liquor A consolidated material again with step (1) in the caustic dolomite ash breast of gained with the mass ratio of 1:1, react generation calcium-magnesium precipitation of hydroxide thing.
By step calcium-magnesium precipitation of hydroxide thing (5) after filtration, washing after, at 800 ℃ of light-burned one-tenth rhombspar magnesia primary raw materialss, and obtain wash water and mother liquor B; Wash water is sent to digestion caustic dolomite, and mother liquor B sends to processing water resistant additive or calcium chloride.
By step primary raw materials (6) under 200MPa pressure, be pressed into the brick body of 300 * 150 * 100mm, then dead roasting in the high temperature kiln of 1600 ℃, obtains rhombspar magnesia.
embodiment 6by bischofite and dolomite made, for a method for rhombspar magnesia, comprised the following steps:
(1) the rhombspar of 980 ℃ of calcinings is ground to form to 180 object rhombspar powder; Get 100 grams of these rhombspar powder and put into beaker, and 800 grams of calcium chloride solutions are joined and in the above-mentioned beaker that fills rhombspar powder, at 30 ℃ ~ 40 ℃ temperature, are digested to caustic dolomite ash breast.
Wherein: in calcium chloride solution, calcium chloride mass content is 20%.
(2) prepare magnesium chloride solution: it is 1.23g/cm that bischofite water is dissolved into proportion
3magnesium chloride solution.
(3) 800 grams of magnesium chloride solutions being joined in the newborn beaker of above-mentioned caustic dolomite ash, and this beaker is placed in to HH-S6 type thermostat water bath, is stirring reaction under the condition of 200 revs/min of 20 ℃, rotating speed at bath temperature, after 5 minutes, generates magnesium hydrate precipitate.
(4) magnesium hydrate precipitate is carried out to countercurrent washing with the water of its 0.5 times of quality, then carry out suction filtration, obtain filter cake and wash water and mother liquor A; Filter cake is dried to constant weight and after 500 ~ 600 ℃ of temperature lower calcinations, is obtained magnesium cement magnesium oxide; Wash water and mother liquor A consolidated material be the raw material for magnesia as the supply system.
By step wash water in (4) and mother liquor A consolidated material again with step (1) in the caustic dolomite ash breast of gained with the mass ratio of 1:1, react generation calcium-magnesium precipitation of hydroxide thing.
By step calcium-magnesium precipitation of hydroxide thing (5) after filtration, washing after, at 800 ℃ of light-burned one-tenth rhombspar magnesia primary raw materialss, and obtain wash water and mother liquor B; Wash water is sent to digestion caustic dolomite, and mother liquor B sends to processing water resistant additive or calcium chloride.
By step primary raw materials (6) under 200MPa pressure, be pressed into the brick body of 300 * 150 * 100mm, then dead roasting in the high temperature kiln of 1600 ℃, obtains rhombspar magnesia.
embodiment 7by bischofite and dolomite made, for a method for rhombspar magnesia, comprised the following steps:
(1) the rhombspar of 980 ℃ of calcinings is ground to form to 180 object rhombspar powder; Get 100 grams of these rhombspar powder and put into beaker, and 400 grams of calcium chloride solutions are joined and in the above-mentioned beaker that fills rhombspar powder, at 30 ℃ ~ 40 ℃ temperature, are digested to caustic dolomite ash breast.
Wherein: in calcium chloride solution, calcium chloride mass content is 15%.
(2) prepare magnesium chloride solution: it is 1.23g/cm that bischofite water is dissolved into proportion
3magnesium chloride solution.
(3) 400 grams of magnesium chloride solutions being joined in the newborn beaker of above-mentioned caustic dolomite ash, and this beaker is placed in to HH-S6 type thermostat water bath, is stirring reaction under the condition of 100 revs/min of 60 ℃, rotating speed at bath temperature, after 30 minutes, generates magnesium hydrate precipitate.
(4) magnesium hydrate precipitate is carried out to countercurrent washing with the water of its 0.5 times of quality, then carry out suction filtration, obtain filter cake and wash water and mother liquor A; Filter cake is dried to constant weight and after 500 ~ 600 ℃ of temperature lower calcinations, is obtained magnesium cement magnesium oxide; Wash water and mother liquor A consolidated material be the raw material for magnesia as the supply system.
By step wash water in (4) and mother liquor A consolidated material again with step (1) in the caustic dolomite ash breast of gained with the mass ratio of 1:1, react generation calcium-magnesium precipitation of hydroxide thing.
By step calcium-magnesium precipitation of hydroxide thing (5) after filtration, washing after, at 800 ℃ of light-burned one-tenth rhombspar magnesia primary raw materialss, and obtain wash water and mother liquor B; Wash water is sent to digestion caustic dolomite, and mother liquor B sends to processing water resistant additive or calcium chloride.
By step primary raw materials (6) under 200MPa pressure, be pressed into the brick body of 300 * 150 * 100mm, then dead roasting in the high temperature kiln of 1600 ℃, obtains rhombspar magnesia.
Claims (1)
- By bischofite and dolomite made for a method for rhombspar magnesia, comprise the following steps:(1) the rhombspar of 900 ℃ ~ 1000 ℃ of calcinings is ground to form to 180 object rhombspar powder, this rhombspar powder is digested to caustic dolomite ash breast with the calcium chloride solution of 3 ~ 8 times of its quality; In described calcium chloride solution, calcium chloride mass content is 1% ~ 20%; The temperature of digestion reaction is 30 ℃ ~ 40 ℃;(2) prepare magnesium chloride solution: it is 1.19 ~ 1.23g/cm that bischofite water is dissolved into proportion 3magnesium chloride solution;(3) the stirring reaction in 20 ℃ ~ 60 ℃ waters bath with thermostatic control by described magnesium chloride solution and described caustic dolomite ash breast, generated magnesium hydrate precipitate after 5 ~ 30 minutes; The mass ratio of wherein said magnesium chloride solution and described calcium chloride solution is 1:0.5 ~ 1; Stirring velocity is 100 ~ 200 revs/min;(4) described magnesium hydrate precipitate is washed with the water of its 0.3 ~ 0.5 times of quality, then carry out suction filtration, obtain filter cake and wash water and mother liquor A; Described filter cake is dried to constant weight and after 500 ~ 600 ℃ of temperature lower calcinations, is obtained magnesium cement magnesium oxide; A described wash water and mother liquor A consolidated material be the raw material for magnesia as the supply system; Mode of washing is countercurrent washing;By described step wash water in (4) and mother liquor A consolidated material again with described step (1) in the caustic dolomite ash breast of gained with the mass ratio of 1:1, react generation calcium-magnesium precipitation of hydroxide thing;By described step calcium-magnesium precipitation of hydroxide thing (5) after filtration, washing after, at 700 ~ 800 ℃ of light-burned one-tenth rhombspar magnesia primary raw materialss, and obtain wash water and mother liquor B; Described wash water is sent to digestion caustic dolomite, and described mother liquor B sends to processing water resistant additive or calcium chloride;By described step primary raw materials (6) under 100MPa ~ 200MPa pressure, be pressed into the brick body of 300 * 150 * 100mm, then dead roasting in the high temperature kiln of 1500 ~ 1600 ℃, obtains rhombspar magnesia.
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| CN201210066762.2A CN102617054B (en) | 2012-03-14 | 2012-03-14 | Method for preparing dolomite magnesia from bischofite and dolomite |
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| CN201210066762.2A CN102617054B (en) | 2012-03-14 | 2012-03-14 | Method for preparing dolomite magnesia from bischofite and dolomite |
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| CN103601224B (en) * | 2013-11-28 | 2015-06-10 | 中国科学院青海盐湖研究所 | Preparation method for magnesium hydroxide |
| CN114573009A (en) * | 2022-01-17 | 2022-06-03 | 南京宝淳新材料科技有限公司 | Method for preparing silicon steel magnesia by using dolomite and bischofite as raw materials |
| CN115611533B (en) * | 2022-09-09 | 2023-08-11 | 中国科学院青海盐湖研究所 | Method for preparing magnesium oxide by stratified isolated calcination of bischofite-dolomite |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1618998A (en) * | 2003-11-20 | 2005-05-25 | 中南大学 | Method of preparing high purity magnesiun sand using salt lake bischofite as raw material |
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| CN1618998A (en) * | 2003-11-20 | 2005-05-25 | 中南大学 | Method of preparing high purity magnesiun sand using salt lake bischofite as raw material |
Non-Patent Citations (2)
| Title |
|---|
| 氧化镁的发展趋势及其生产方法;高洁等;《化工生产与技术》;20050531(第5期);第37页第3部分 * |
| 高洁等.氧化镁的发展趋势及其生产方法.《化工生产与技术》.2005,(第5期),第37页第3部分. |
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