CN102079522A - Method for improving extraction efficiency of silicon - Google Patents
Method for improving extraction efficiency of silicon Download PDFInfo
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- CN102079522A CN102079522A CN 201010566643 CN201010566643A CN102079522A CN 102079522 A CN102079522 A CN 102079522A CN 201010566643 CN201010566643 CN 201010566643 CN 201010566643 A CN201010566643 A CN 201010566643A CN 102079522 A CN102079522 A CN 102079522A
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Abstract
The invention discloses a method for improving the extraction efficiency of silicon. The method comprises the following steps of: grinding a raw material until the particle size of the raw material is between 1 and 2 millimeters; uniformly mixing the ground material and NaOH, putting the mixture into a high-pressure reaction kettle, adding water and reacting for 1 to 5 hours by controlling the reaction temperature of the high-pressure reaction kettle to be between 250 and 420 DEG C, the reaction pressure intensity at 0.2 MPa and internal stirring speed of the kettle at 500 revolutions per minute; and opening a kettle body cooling system, cooling to room temperature, filtering and separating so as to obtain silicon liquid. The method has high efficiency, low energy consumption, low time consumption and simple and convenient process, is easy to control and does not cause environmental pollution; and a product can be widely applied to industries such as aviation and aerospace, electronics and electricity, construction, transportation, chemical industry, textile, foods, light industry, medical treatment and the like.
Description
(1) technical field the present invention relates to silicon, designs a kind of method that improves the extraction efficiency of silicon especially.
(2) the background technology crystalline silicon is a grey black, belongs to atomic crystal, firmly metalluster is arranged, and semiconductor property is arranged.The chemical property of silicon is more active, at high temperature can with multiple element chemical combination such as oxygen, water insoluble, nitric acid and hydrochloric acid, be dissolved in hydrofluoric acid and alkali lye, be used for alloying such as ferrosilicon, silicon steel etc., silicon single crystal is a kind of important semiconductor material, is used to make high power transistor, rectifier, solar cell etc.
Silicate slag, mine tailing, etc. indissoluble mineral or glass be very typical solid refuse of current China one class, general at present as producing cement.Because the peculiar glass reticulated structure of silicate has good chemical stability, be difficult to utilize metallurgical method of tradition and principle directly therefrom silicate slag, mine tailing, etc. extract silicon in indissoluble mineral or the glass.At present therefrom silicate slag, mine tailing, etc. when extracting silicon in indissoluble mineral or the glass, general earlier it mixing with solid sodium hydroxide, be heated to certain temperature then as 600 ℃ of slaking for some time, carry out lixiviate with water as solvent again.Compare with the direct extraction of sodium hydroxide solution, get efficient although this method can improve to a certain extent, its extraction efficiency is still lower, the temperature height, and energy consumption is big, and needs one to two day time.These methods all can not solve well silicate slag, mine tailing, etc. the extraction problem of silicon in indissoluble mineral or the glass.
Recently studies show that subcritical or supercritical water can be smashed the glass particle in the flying dust, promptly subcritical or supercritical water has crushing effect to glass particle; In addition, under subcritical or super critical condition, water molecules is diffused at an easy rate in the glass to react with its alkalimetal oxide (Si-O-Na+) and forms OH-ion (Si-OH+Na++OH-), and OH-can make the ≡ Si-O-Si ≡ key of glass network that fracture takes place and generate (Si-OH+Na+O-Si).Therefore, subcritical or supercritical water can destroy the reticulated structure of glass effectively.
(3) summary of the invention
1, goal of the invention; Purpose of the present invention is intended to overcome above-mentioned deficiency of the prior art, provide a kind of from silicate slag, mine tailing, etc. the method for rapid extraction silicon indissoluble mineral or the glass.
2, technical scheme: technical scheme of the present invention is: a kind of method that improves the extraction efficiency of silicon in turn includes the following steps: with raw material crushing to particle diameter 1～2mm; Itself and NaOH are mixed again, put into autoclave, add entry, control autoclave temperature of reaction is 250-420 ℃, and stirring velocity is 500r/min in the reaction pressure 0.2MPa, still, reaction 1-5h; Open the kettle cooling system, be cooled to room temperature, filtering separation obtains silicon liquid.
3, beneficial effect: compared with prior art, the present invention has following characteristics and beneficial effect: 1. the present invention with silicate slag, mine tailing, etc. indissoluble mineral or glass be raw material, adopt Asia/supercritical water-NaOH extraction process, it is low to have overcome in the conventional extraction silicon process efficient, energy consumption is big, defectives such as length consuming time prepare silicon; The result shows that the extraction yield of silicon is 86.54%; 2. technological operation easy, be easy to control, production cost is low, and technological process environmentally safe; 3. technology to the silicate slag, mine tailing of preparation silicon, etc. indissoluble mineral or component of glass raw material do not have strict demand, applied widely; Prepared product can be widely used in industries such as aerospace, electric, building, transportation, chemical industry, weaving, food, light industry, medical treatment, has broad application prospects.
(4) the description of drawings Figure of description is a process flow sheet of the present invention.
(5) below the embodiment be several concrete embodiment of the present invention.The invention is not restricted to these embodiment.
Embodiment 1: with electronic waste color cathod-ray display screen glass is raw material, with mechanical crushing method it is crushed to about 1～3cm earlier, further is crushed to particle diameter less than 0.5mm with planetary ball mill again.Get 5g glass powder, add 5gNaOH and mix, put into the autoclave of 200mL, add 120mL water.Control autoclave temperature of reaction is 420 ℃, and stirring velocity is 500r/min in the reaction pressure 0.2MPa, still, reaction 1h; Open the kettle cooling system, be cooled to room temperature, filtering separation is with the distribution of silicon in sample before inductively-coupled plasma spectrometer (OPTIMA 2000) analytical solution and the reaction and the reaction back residue (solid adopts the HNO3/HClO4/HF method to clear up).The result shows that the extraction yield of silicon is 86.54%, and its concentration is 9.65g/L.
Embodiment 2: getting plasma display glass is raw material, and coarse breaking is crushed to particle diameter 1～2mm with planetary ball mill again to about 1～3cm.Get 5g glass powder, add 10g NaOH and mix, put into the autoclave of 200mL, add 120mL water, control autoclave temperature of reaction is 300 ℃, and stirring velocity is 500r/min in the reaction pressure 0.2MPa, still, reaction 3h; Open the kettle cooling system, be cooled to room temperature, filtering separation obtains silicon liquid.
Embodiment 3: with the silicate slag is raw material, with mechanical crushing method it is crushed to about 1～3cm earlier, further is crushed to particle diameter 0.5～1mm with planetary ball mill again.Get the 5g slag, add 20g NaOH and mix, put into the autoclave of 200mL, add 120mL water.Control autoclave temperature of reaction is 250 ℃, and stirring velocity is 500r/min in the reaction pressure 0.2MPa, still, reaction 5h; Open the kettle cooling system, be cooled to room temperature, filtering separation obtains silicon liquid.
Claims (1)
1. method that improves the extraction efficiency of silicon in turn includes the following steps: with raw material crushing to particle diameter 1～2mm; Itself and NaOH are mixed again, put into autoclave, add entry, control autoclave temperature of reaction is 250-420 ℃, and stirring velocity is 500r/min in the reaction pressure 0.2MPa, still, reaction 1-5h; Open the kettle cooling system, be cooled to room temperature, filtering separation obtains silicon liquid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010566643 CN102079522A (en) | 2010-12-01 | 2010-12-01 | Method for improving extraction efficiency of silicon |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN 201010566643 CN102079522A (en) | 2010-12-01 | 2010-12-01 | Method for improving extraction efficiency of silicon |
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| CN102079522A true CN102079522A (en) | 2011-06-01 |
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| CN 201010566643 Pending CN102079522A (en) | 2010-12-01 | 2010-12-01 | Method for improving extraction efficiency of silicon |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106525561A (en) * | 2016-11-03 | 2017-03-22 | 芜湖东旭光电科技有限公司 | Method for determining content of platinum and rhodium in glass |
| CN110272058A (en) * | 2019-07-01 | 2019-09-24 | 中南大学 | A kind of MCM-41 ordered mesoporous material and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101613802A (en) * | 2009-07-13 | 2009-12-30 | 中国科学院生态环境研究中心 | The technology of reclaiming lead and producing environment-friendly building material by waste flint glass and support equipment |
-
2010
- 2010-12-01 CN CN 201010566643 patent/CN102079522A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101613802A (en) * | 2009-07-13 | 2009-12-30 | 中国科学院生态环境研究中心 | The technology of reclaiming lead and producing environment-friendly building material by waste flint glass and support equipment |
Non-Patent Citations (1)
| Title |
|---|
| 《Journal of Hazardous Materials》 20100604 Mengjun Chen,et al. Effective utilization of waste cathode ray tube glass-Crystalline silicotitanate synthesis 第182卷, * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106525561A (en) * | 2016-11-03 | 2017-03-22 | 芜湖东旭光电科技有限公司 | Method for determining content of platinum and rhodium in glass |
| CN110272058A (en) * | 2019-07-01 | 2019-09-24 | 中南大学 | A kind of MCM-41 ordered mesoporous material and preparation method thereof |
| CN110272058B (en) * | 2019-07-01 | 2022-08-09 | 中南大学 | MCM-41 ordered mesoporous material and preparation method thereof |
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Application publication date: 20110601 |