WO2014183380A1 - 碳化硅滤饼旋流提纯工艺 - Google Patents
碳化硅滤饼旋流提纯工艺 Download PDFInfo
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- WO2014183380A1 WO2014183380A1 PCT/CN2013/085458 CN2013085458W WO2014183380A1 WO 2014183380 A1 WO2014183380 A1 WO 2014183380A1 CN 2013085458 W CN2013085458 W CN 2013085458W WO 2014183380 A1 WO2014183380 A1 WO 2014183380A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- silicon carbide
- filter cake
- suspension
- cyclone
- silicon
- Prior art date
Links
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 63
- 239000012065 filter cake Substances 0.000 title claims abstract description 32
- 238000000746 purification Methods 0.000 title claims abstract description 13
- 238000000034 method Methods 0.000 title claims abstract description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 27
- 239000000725 suspension Substances 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000011085 pressure filtration Methods 0.000 claims description 7
- JTJMJGYZQZDUJJ-UHFFFAOYSA-N phencyclidine Chemical class C1CCCCN1C1(C=2C=CC=CC=2)CCCCC1 JTJMJGYZQZDUJJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000013049 sediment Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 1
- 239000004570 mortar (masonry) Substances 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- 239000002699 waste material Substances 0.000 description 6
- 239000003513 alkali Substances 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000005484 gravity Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000002173 cutting fluid Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000005554 pickling Methods 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- XUIMIQQOPSSXEZ-NJFSPNSNSA-N silicon-30 atom Chemical compound [30Si] XUIMIQQOPSSXEZ-NJFSPNSNSA-N 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/956—Silicon carbide
Definitions
- the invention relates to the technical field of solid-liquid separation of waste mortar, in particular to a method for obtaining silicon carbide filter cake after solid-liquid separation from single crystal silicon slice waste sand slurry, and then purifying silicon carbide by a swirling process.
- the waste mortar mainly contains silicon carbide, polyethylene glycol cutting fluid, silicon powder, etc., and the waste mortar is subjected to solid-liquid separation by a filter press to obtain a silicon carbide filter cake (mainly containing silicon carbide, silicon powder, carbon, etc.).
- the silicon carbide filter cake generally has a silicon carbide content of 80%, a silicon powder content of 15%, a carbon content of 3.5%, and other impurities of 1.5%.
- the main processes for chemical purification according to the traditional process are: alkaline washing, water washing, pickling, and water washing.
- alkali washing sodium hydroxide is added to react with silicon powder to form sodium silicate and a large amount of hydrogen.
- the process has certain dangers and high pollution, and a large amount of hydrogen gas may cause hydrogen explosion; the water after alkali washing is Black, large amount of water for cleaning, a large amount of black sewage is difficult to handle, discharged into the natural environment, seriously affecting water quality and soil quality.
- the invention adopts silicon carbide filter cake as raw material, and is mixed with water, sieved by vibrating sieve, separated by cyclone separation, and centrifuged to obtain coarse silicon carbide; the waste is subjected to pressure filtration to obtain coarse silicon powder.
- a silicon carbide filter cake cyclone purification process the process steps are as follows:
- the silicon carbide filter cake and water are mixed at a weight ratio of 2:3, and stirred evenly; (2) The silicon carbide filter cake suspension is sieved through a 200 mesh vibrating screen;
- the upper silicon powder suspension obtained in the step (3) is subjected to pressure filtration to obtain a wet crude silicon powder.
- the silicon carbide filter cake in the step (1) is mixed with water and stirred until no sediment appears.
- the content of silicon carbide in the crude silicon carbide is 96-97%.
- the content of the silicon powder in the coarse silicon powder is 60% or more.
- the beneficial effects of the present invention are as follows: Compared with the prior art, the present invention is directed to the defects of the conventional process, the cyclone pretreatment of the silicon carbide filter cake, and the coarse separation of the swirling flow by using the different specific gravity of the silicon carbide, the silicon powder and the carbon, The silicon carbide content in the silicon carbide filter cake is increased from 80% to 96-97%, and the silicon powder content of the silicon powder waste by pressure filtration is more than 60%, and the silicon powder can be further purified; the subsequent alkali washing and pickling can be reduced. With alkali, acid and clean water, the wastewater is not black, the sewage treatment is simple, it does not affect the environment, and the production cycle is greatly shortened.
- the cyclone purification process of the present invention removes most of the silicon powder in the silicon carbide filter cake according to the specific gravity of the silicon carbide and the silicon powder, thereby greatly reducing the amount of alkali, acid and water in the subsequent chemical purification of the silicon carbide. Shorten production cycles and reduce environmental pollution.
- the silicon carbide filter cake is purified by mixing with water, sieving, swirling, centrifuging, and pressure filtration.
- the silicon carbide filter cake suspension is passed through a 200 mesh ultrasonic vibrating screen to remove large particle impurities in the suspension.
- the silicon carbide filter cake suspension is sequentially introduced into the 1, 2, and 3 sets of cyclones for swirling.
- the variable frequency mortar pump is used to transport the suspension to the cyclone to form a swirling vortex.
- the silicon carbide and silicon powder have different specific gravity, the silicon carbide suspension is discharged from the lower overflow port, and the silicon powder suspension is discharged from the overflow nozzle to maintain the swirling flow. 2MPa ⁇
- the pressure is 0. 18-0. 2MPa.
- the silicon carbide suspension from the overflow port of the No. 3 cyclone enters the buffer tank and can be centrifuged.
- the silicon powder suspension of the overflow port is again swirled through the 4 and 5 cyclones to maintain the same pressure 0. 18-0. 2MPa, wherein the silicon powder suspension from the overflow of the cyclone No. 5 After entering the buffer tank, the next pressure filtration process is performed; the silicon carbide suspension of the underflow outlet is returned to the No. 1 cyclone for swirling again.
- the silicon carbide suspension is centrifuged to obtain 950 kg of crude wet silicon carbide, which has a moisture content of 12%, a silicon carbide content of 96.6% (on a dry basis), a silicon powder content of 2%, a carbon content of 1%, and the like. 4% ⁇ The impurity content of 0. 4%.
- the silica powder suspension is subjected to pressure filtration by a plate and frame filter press to obtain 300 kg of crude wet silicon powder, 18% of which is tested for moisture, 68% of silicon powder, and 30% of silicon carbide fine powder (particle size 4 ⁇ ⁇ ).
Abstract
提供一种碳化硅滤饼旋流提纯工艺，包括：（1）碳化硅滤饼与水按重量比2：3混合搅拌均匀；（2）碳化硅滤饼悬浮液振动经过200目筛；（3）将碳化硅滤饼悬浮液输入旋流器进行旋流；（4）将步骤（3）获得的下层碳化硅悬浮液经离心后得到湿粗碳化硅；（5）将步骤（3）获得的上层硅粉悬浮液经压滤后得到湿粗硅粉。
Description
碳化硅滤饼旋流提纯工艺 技术领域
本发明涉及废砂浆的固液分离技术领域，尤其是一种从单晶硅切片废砂 浆中经固液分离后，得到碳化硅滤饼，然后采用旋流工艺提纯碳化硅的方法。 背景技术
碳化硅 （微粉级） 与聚乙二醇切削液按 5: 5混合后， 形成碳化硅悬浮 砂浆， 对光伏产品单 （多） 晶硅棒进行切割， 经切割后， 该砂浆可以进行回 收利用， 避免影响环境。 废砂浆中主要含有碳化硅、 聚乙二醇切削液、 硅粉 等， 该废砂浆经过压滤机固液分离后， 得到碳化硅滤饼 （主要含有碳化硅、 硅粉、 碳等）。
碳化硅滤饼一般碳化硅含量 80%、 硅粉含量 15%、 碳含量 3. 5%、 其他杂 质 1. 5%。 按传统工艺化学提纯主要工艺为， 碱洗、 水洗、 酸洗、 水洗。 其中 碱洗时投入氢氧化钠， 与硅粉反应， 生成硅酸钠和大量氢气， 该工艺有一定 危险性和高污染性， 产生的大量氢气有可能会引起氢气爆炸； 碱洗后的水为 黑色、 清洗用水量大， 大量黑色污水难以处理， 排入自然环境中， 严重影响 水质和土质。
发明内容
本发明的目的是提供一种碳化硅滤饼旋流提纯工艺方法， 适合工业规模 化生产。 本发明采用以碳化硅滤饼为原料， 经过加水混合、 振动筛过筛、 旋 流分离提纯、 离心， 得到粗碳化硅； 废弃物经压滤后得到粗硅粉。
本发明的目的是通过采用以下技术方案来实现的：
碳化硅滤饼旋流提纯工艺， 所述工艺步骤如下：
( 1 ) 碳化硅滤饼与水按重量比 2 : 3进行混合， 搅拌均匀；
(2 ) 碳化硅滤饼悬浮液经过 200目振动筛振动过筛；
(3 ) 旋流， 将碳化硅滤饼悬浮液输送进入旋流器， 进行旋流；
(4) 将步骤 （3 ) 获得的下层碳化硅悬浮液经离心后， 得到湿粗碳化硅；
(5 ) 将步骤 （3 ) 获得的上层硅粉悬浮液经压滤后， 得到湿粗硅粉。
作为本发明的优选技术方案， 所述步骤 （1 ) 中碳化硅滤饼与水混合搅 拌至无沉降物出现。
作为本发明的优选技术方案， 所述步骤 （3 ) 碳化硅悬浮液经过 5组旋 流器旋流， 旋流器中压力为 0. 18-0. 2MPa。
作为本发明的优选技术方案， 所述粗碳化硅中碳化硅的含量为 96-97%。 作为本发明的优选技术方案， 所述粗硅粉中硅粉的含量为 60%以上。 本发明的有益效果是： 相对于现有技术， 本发明针对传统工艺的缺陷， 对碳化硅滤饼进行旋流预处理， 利用碳化硅、 硅粉和碳的比重不同， 进行旋 流粗分离， 将碳化硅滤饼中碳化硅含量从 80%提升至 96-97%, 压滤出的硅粉 废弃物硅粉含量 60%以上， 可以进行硅粉再提纯； 后道碱洗、 酸洗可以减少 用碱、 酸、 清水量， 废水不为黑色， 污水处理简单， 不影响环境， 大大缩短 生产周期。
具体实施方式
本发明旋流提纯工艺是根据碳化硅与硅粉的比重不同， 去除碳化硅滤饼 中的大部分硅粉， 从而在后道化学提纯碳化硅时， 大大减少用碱、 酸、 水的 量， 缩短生产周期， 减少环境污染。 碳化硅滤饼经加水混合、 过筛、 旋流、 离心、 压滤进行提纯。
1、 投料混合在 5000L搅拌釜中依次投入 1500kg水和 1000kg碳化硅滤 饼， 开启搅拌 3-4小时， 直至釜底无沉降物， 形成碳化硅滤饼悬浮液（滤饼 浓度 40%)。
2、 碳化硅滤饼悬浮液经过 200 目超声波振动筛， 去除悬浮液中大颗粒 杂质。
3、 碳化硅滤饼悬浮液依次进入 1、 2、 3组旋流器， 进行旋流。 采用变 频砂浆泵输送悬浮液至旋流器中，形成旋流涡，利用碳化硅、硅粉比重不同， 下溢流口出碳化硅悬浮液， 上溢流口出硅粉悬浮液， 保持旋流器中压力为 0. 18-0. 2MPa。 3号旋流器下溢流口出的碳化硅悬浮液进入缓冲釜中，可以进 行离心。 上溢流口的硅粉悬浮液再次经过 4、 5号旋流器进行旋流， 保持同 样的压力 0. 18-0. 2MPa， 其中 5号旋流器上溢流口出的硅粉悬浮液进入缓冲 罐中， 进行下道压滤工序； 下溢流口的碳化硅悬浮液返回 1号旋流器再次进 行旋流。
4、碳化硅悬浮液进行离心机离心， 得到湿碳化硅粗品 950kg， 经检测水 分 12%, 碳化硅含量 96. 6% (按干品计）、 硅粉含量 2%、 碳含量 1%、 其他杂 质含量 0. 4%。
5、硅粉悬浮液进行板框压滤机压滤， 得到湿硅粉粗品 300kg， 经检测水 分 18%, 硅粉含量 68%, 碳化硅细粉 （粒径 4 μ πι) 含量 30%。
Claims
1、 一种碳化硅滤饼旋流提纯工艺， 其特征是所述工艺步骤如下：
( 1 ) 碳化硅滤饼与水按重量比 2 : 3进行混合， 搅拌均匀；
(2 ) 碳化硅滤饼悬浮液经过 200目振动筛振动过筛；
(3 ) 旋流， 将碳化硅滤饼悬浮液输送进入旋流器， 进行旋流；
(4) 将步骤 （3 ) 获得的下层碳化硅悬浮液经离心后， 得到湿粗碳化硅；
(5 ) 将步骤 （3 ) 获得的上层硅粉悬浮液经压滤后， 得到湿粗硅粉。
2、 根据权利要求 1所述的碳化硅滤饼旋流提纯工艺， 其特征是： 所述 步骤 （1 ) 中碳化硅滤饼与水混合搅拌至无沉降物出现。
3、 根据权利要求 1所述的碳化硅滤饼旋流提纯工艺， 其特征是： 所述 步骤（3 )碳化硅悬浮液经过 5组旋流器旋流，旋流器中压力为 0. 18-0. 2MPa。
4、 根据权利要求 1所述的碳化硅滤饼旋流提纯工艺， 其特征是： 所述 粗碳化硅中碳化硅的含量为 96-97%。
5、 根据权利要求 1所述的碳化硅滤饼旋流提纯工艺， 其特征是： 所述 粗硅粉中硅粉的含量为 60%以上。
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| CN103232039A (zh) * | 2013-05-16 | 2013-08-07 | 周彬 | 碳化硅滤饼旋流提纯工艺 |
| CN103539123A (zh) * | 2013-10-25 | 2014-01-29 | 宁夏机械研究院（有限责任公司） | 亚微米级碳化硅微粉的酸洗提纯方法 |
| CN103922343B (zh) * | 2014-03-19 | 2016-03-09 | 河南易成新能源股份有限公司 | 碳化硅切割刃料除铁提纯方法 |
| CN103922342B (zh) * | 2014-03-19 | 2016-08-17 | 河南易成新能源股份有限公司 | 碳化硅微粉旋流提纯方法 |
| CN105948055B (zh) * | 2016-05-30 | 2017-12-22 | 山田研磨材料有限公司 | 半导体用高纯碳化硅微粉的提纯方法 |
| CN106335902B (zh) * | 2016-08-24 | 2019-02-19 | 山田研磨材料有限公司 | 一种碳化硅微粉的回收方法 |
| CN109160759B (zh) * | 2018-10-12 | 2021-04-20 | 中水电第十一工程局（郑州）有限公司 | 一种硅粉悬浮液的制备方法 |
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- 2013-05-16 CN CN2013101874643A patent/CN103232039A/zh active Pending
- 2013-10-18 WO PCT/CN2013/085458 patent/WO2014183380A1/zh active Application Filing
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