CN102328930A - Method for recovering silicon carbide from waste mortar from monocrystalline silicon slicing - Google Patents
Method for recovering silicon carbide from waste mortar from monocrystalline silicon slicing Download PDFInfo
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- CN102328930A CN102328930A CN201110210863A CN201110210863A CN102328930A CN 102328930 A CN102328930 A CN 102328930A CN 201110210863 A CN201110210863 A CN 201110210863A CN 201110210863 A CN201110210863 A CN 201110210863A CN 102328930 A CN102328930 A CN 102328930A
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- silit
- silicon carbide
- waste mortar
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Abstract
The invention discloses a method for recovering silicon carbide from waste mortar from monocrystalline silicon slicing, which comprises the following steps: 1, selecting waste mortar from monocrystalline silicon slicing, mixing with water, heating, and separating with a centrifuge to obtain silicon carbide filter cakes; 2, placing the silicon carbide filter cakes in a 10% sodium hydroxide solution, and carrying out alkali wash; 3, placing the silicon carbide filter cakes subjected to alkali wash in a mixed solution of hydrofluoric acid and 20% sulfuric acid, and carrying out acid wash; 4, placing the silicon carbide filter cakes subjected to acid wash in a mixed solution of water and kerosene, and decarbonizing to obtain wet pure silicon carbide products; and 5, finally fast drying the wet pure silicon carbide products to obtain dry silicon carbide products. The silicon carbide recovery method provided by the invention is applicable to industrial large-scale production, is beneficial to the cyclic development and cost saving of production, and reduces the pollution of industrial waste to the environment.
Description
Technical field
The present invention relates to a kind of method that from silicon single crystal section waste mortar, reclaims silit.
Background technology
Silit (SiC) is to be that raw material forms through the resistance furnace pyrotic smelting with silica sand, refinery coke (or coal tar), wood chip, and also there is unusual mineral in silit at the Nature, and Mo Sangshi, silit claim moissanite again.In non-oxidized substance hi-tech refractory raw materials such as contemporary C, N, B, silit is extensive, the most most economical a kind of for using.Can be called powder emery or fire sand, silit is to form through pyrotic smelting in resistance furnace with raw materials such as silica sands, refinery coke (or coal tar), wood chip (when producing green silicon carbide need with salt).At present the industrial silit of China is divided into two kinds of black silicon carbide and green silicon carbides, is hexagonal, and proportion is 3.20～3.25, and microhardness is 2840～3320kg/mm2.The purposes of silit: (1) can be used to do grinding tool as abrasive material, like emery wheel, oilstone, bistrique, grinding segment class etc.; (2) as metallurgical reductor and high temperature material; Silit mainly contains four big Application Areass; That is: function ceramics, high grade refractory, abrasive material and metallurgical raw material; At present the silit coarse fodder can be supplied in a large number, can not calculate new high-tech product, and the application short period of time of the high nano-grade silicon carbide powder of technology content can not form scale economics; (3) highly purified monocrystalline can be used for making semi-conductor, makes silicon carbide fiber.Its main application: be used for line cuttings such as 3-12 inch silicon single crystal, polysilicon, arsenic potassium, quartz crystal, photovoltaic industry, semiconductor industry, piezoquartz industry engineering property work material.Flourish along with this new industry of photovoltaic industry, the market demand of silit is also increasing, the recycling of the useless slurry of silit, cost is practiced thrift in the cycle development that helps producing, and reduces the trade waste pollution on the environment.
Summary of the invention
The invention provides a kind of method that from silicon single crystal section waste mortar, reclaims silit, be fit to industrial-scale production, help the cycle development of producing simultaneously, practice thrift cost, and reduce the trade waste pollution on the environment.
The present invention has adopted following technical scheme: a kind of method that from silicon single crystal section waste mortar, reclaims silit; May further comprise the steps: step 1; Select silicon single crystal section waste mortar and mixes, heat up then and use the whizzer separation, obtain the silit filter cake with water; Step 2 is put into 10% sodium hydroxide solution with the silit filter cake and is carried out alkali cleaning; Step 3 is put into hydrofluoric acid and 20% vitriolic mixing solutions carries out pickling with the silit filter cake after the alkali cleaning; Step 4, the mixing solutions of the silit filter cake after the pickling being put into water and kerosene carries out de-carbon, obtains the wet article of pure silit; Step 5 is carried out flash baking to the wet article of pure silit at last, obtains the silit dry product.
The mass ratio of waste mortar and water is 1: 0.5 in the said step 1, uses whizzer to separate after being warming up to 40 ℃; The mass ratio of silit filter cake and 10% sodium hydroxide solution is 1: 1.2 in the said step 2, and the alkali cleaning temperature is 60 ℃; Silit filter cake and hydrofluoric acid and 20% vitriolic mass ratio are 1: 0.01: 0.7 in the said step 3, and pickling temperature is 60 ℃; The mass ratio of silit filter cake and water and kerosene is 1: 2: 0.001 in the said step 4; Utilize the flash distillation machine to carry out flash baking in the said step 5,250 ℃ of flash distillation EATs, 120 ℃ of drop temperatures.
The present invention has following beneficial effect: the method for recovery silit provided by the invention, be fit to industrial-scale production, and help the cycle development of producing simultaneously, practice thrift cost, and reduce the trade waste pollution on the environment.
Embodiment
The invention provides a kind of method that from silicon single crystal section waste mortar, reclaims silit; May further comprise the steps: step 1, to select silicon single crystal section waste mortar and mix with water, the mass ratio of waste mortar and water is 1: 0.5; Be warming up to 40 ℃ and use whizzer to separate then, obtain the silit filter cake;
Step 2 is put into 10% sodium hydroxide solution with the silit filter cake and is carried out alkali cleaning, and the mass ratio of silit filter cake and 10% sodium hydroxide solution is 1: 1.2, and the alkali cleaning temperature is 60 ℃;
Step 3 is put into hydrofluoric acid and 20% vitriolic mixing solutions carries out pickling with the silit filter cake after the alkali cleaning, and silit filter cake and hydrofluoric acid and 20% vitriolic mass ratio are 1: 0.01: 0.7, and pickling temperature is 60 ℃;
Step 4, at normal temperatures, the mixing solutions of the silit filter cake after the pickling being put into water and kerosene carries out de-carbon, obtains the wet article of pure silit, and the mass ratio of silit filter cake and water and kerosene is 1: 2: 0.001;
Step 5 utilizes the flash distillation machine that the wet article of pure silit are carried out flash baking at last, 250 ℃ of flash distillation EATs, and 120 ℃ of drop temperatures obtain the silit dry product at last.
Embodiment
With the 1200# waste mortar is example
1, solid-liquid separation
In 5000L jacketed reaction kettle, drop into 2000kg waste mortar and 1000kg water; Feed in the chuck and be steam heated to 40 ℃, stirred 30 minutes, make useless slurry of cutting fluid and water thorough mixing; Carry out solid-liquid separation at whizzer again, obtain silit filter cake 1200kg and cutting fluid aqueous solution 1800kg.The cutting fluid aqueous solution obtains cutting fluid through decolouring, dehydration, mediation.
2, alkali cleaning
In the 3000L stainless steel cauldron, drop into 1200kg silit filter cake and 10% sodium hydroxide solution 1440kg, the slow heat temperature raising to 60 of steam ℃, and be incubated 2 hours, centrifugal removal liquid must remove a step product light green silit bullion 950kg behind the silica flour.
3, pickling
In the 2000L reaction kettle, one the step product 950kg and 20% sulfuric acid 665kg and hydrofluoric acid 9.5kg, heat temperature raising to 60 ℃ is incubated 4 hours, centrifugally obtains secondary product silit bullion 940kg behind deironing, the Starso.
4, washing de-carbon
In the 3000L reaction kettle, drop into secondary product 940kg and water 1880kg and kerosene 0.94kg, filter screen is installed at the liquid level place, in the whipping process, filter out the carbon dust that is suspended in liquid level, do not have the black suspension thing until liquid level.Centrifugal, obtain the wet article 935kg of pure silit.
5, flash distillation oven dry
The flash distillation machine utilizes heat-conducting oil heating, and intake air temperature transfers to 250 ℃, and wet article 935kg drops into the flash distillation machine in batches with pure silit, and 120 ℃ of discharge port temperature obtain silit dry product 850kg.Detect each item index: carborundum content>=98.5%, free carbon content≤0.5%, iron level≤0.5%, silicon and dioxide-containing silica≤1%.
Claims (6)
1. method that from silicon single crystal section waste mortar, reclaims silit is characterized in that it may further comprise the steps:
Step 1 is selected silicon single crystal section waste mortar and is mixed with water, heats up then and uses the whizzer separation, obtains the silit filter cake;
Step 2 is put into 10% sodium hydroxide solution with the silit filter cake and is carried out alkali cleaning;
Step 3 is put into hydrofluoric acid and 20% vitriolic mixing solutions carries out pickling with the silit filter cake after the alkali cleaning;
Step 4, the mixing solutions of the silit filter cake after the pickling being put into water and kerosene carries out de-carbon, obtains the wet article of pure silit;
Step 5 is carried out flash baking to the wet article of pure silit at last, obtains the silit dry product.
2. a kind of method that from silicon single crystal section waste mortar, reclaims silit according to claim 1 is characterized in that the mass ratio of waste mortar and water is 1: 0.5 in the said step 1, uses the whizzer separation after being warming up to 40 ℃.
3. a kind of method that from silicon single crystal section waste mortar, reclaims silit according to claim 1 is characterized in that the mass ratio of silit filter cake and 10% sodium hydroxide solution is 1: 1.2 in the said step 2, and the alkali cleaning temperature is 60 ℃.
4. a kind of method that from silicon single crystal section waste mortar, reclaims silit according to claim 1 is characterized in that silit filter cake and hydrofluoric acid and 20% vitriolic mass ratio are 1: 0.01: 0.7 in the said step 3, and pickling temperature is 60 ℃.
5. a kind of method that from silicon single crystal section waste mortar, reclaims silit according to claim 1 is characterized in that the mass ratio of silit filter cake and water and kerosene is 1: 2: 0.001 in the said step 4.
6. a kind of method that from silicon single crystal section waste mortar, reclaims silit according to claim 1 is characterized in that utilizing in the said step 5 flash distillation machine to carry out flash baking, 250 ℃ of flash distillation EATs, 120 ℃ of drop temperatures.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110210863A CN102328930A (en) | 2011-07-22 | 2011-07-22 | Method for recovering silicon carbide from waste mortar from monocrystalline silicon slicing |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201110210863A CN102328930A (en) | 2011-07-22 | 2011-07-22 | Method for recovering silicon carbide from waste mortar from monocrystalline silicon slicing |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114314592A (en) * | 2021-12-31 | 2022-04-12 | 常州赛蓝光伏技术有限公司 | Purification method and filtering device for recovering silicon carbide micro powder from waste mortar generated in cutting silicon |
| TWI775612B (en) * | 2021-09-17 | 2022-08-21 | 行政院原子能委員會核能研究所 | Reclamation of silicon carbide from abrasive slurry |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1689718A (en) * | 2004-04-21 | 2005-11-02 | 尹克胜 | Waste sand treating method in crystal processing |
| CN101920959A (en) * | 2009-06-15 | 2010-12-22 | 南京工业大学 | Purification process of silicon carbide micro powder for linear cutting |
-
2011
- 2011-07-22 CN CN201110210863A patent/CN102328930A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1689718A (en) * | 2004-04-21 | 2005-11-02 | 尹克胜 | Waste sand treating method in crystal processing |
| CN101920959A (en) * | 2009-06-15 | 2010-12-22 | 南京工业大学 | Purification process of silicon carbide micro powder for linear cutting |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI775612B (en) * | 2021-09-17 | 2022-08-21 | 行政院原子能委員會核能研究所 | Reclamation of silicon carbide from abrasive slurry |
| CN114314592A (en) * | 2021-12-31 | 2022-04-12 | 常州赛蓝光伏技术有限公司 | Purification method and filtering device for recovering silicon carbide micro powder from waste mortar generated in cutting silicon |
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Application publication date: 20120125 |