WO2014183381A1 - 一种碳化硅滤饼碱洗提纯方法 - Google Patents
一种碳化硅滤饼碱洗提纯方法 Download PDFInfo
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- WO2014183381A1 WO2014183381A1 PCT/CN2013/085460 CN2013085460W WO2014183381A1 WO 2014183381 A1 WO2014183381 A1 WO 2014183381A1 CN 2013085460 W CN2013085460 W CN 2013085460W WO 2014183381 A1 WO2014183381 A1 WO 2014183381A1
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- WO
- WIPO (PCT)
- Prior art keywords
- silicon carbide
- filter cake
- water
- carbide filter
- suspension
- Prior art date
Links
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 55
- 239000012065 filter cake Substances 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 15
- 238000000746 purification Methods 0.000 title claims abstract description 6
- 239000003518 caustics Substances 0.000 title abstract 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 24
- 239000000725 suspension Substances 0.000 claims abstract description 12
- 239000000047 product Substances 0.000 claims abstract description 7
- 239000003513 alkali Substances 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 7
- 238000011085 pressure filtration Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims 2
- 238000004140 cleaning Methods 0.000 claims 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 11
- 239000011863 silicon-based powder Substances 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000004570 mortar (masonry) Substances 0.000 description 5
- 239000002699 waste material Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000002173 cutting fluid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000007787 solid 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 silicon carbide filter cake obtained by solid-liquid separation from a single crystal silicon slice waste sand slurry, and then a method for purifying silicon carbide.
- 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%.
- sodium hydroxide and silicon powder are required to react to remove the silicon powder.
- the conventional process is to put the silicon carbide filter cake into water, and then add sodium hydroxide solids in batches to react, during which a large amount of gas is generated, and the temperature is generated. Up to 120 ° C, boiling state, the material is easily sprayed from the reaction tank or the reaction tank, resulting in material loss; the amount of alkali added is several times the amount of silicon powder, resulting in an increase in production costs, the amount of later washing alkali water, sewage The processing cost is high.
- An object of the present invention is to provide a method for purifying and purifying a silicon carbide filter cake, which is suitable for industrial scale production.
- the invention adopts silicon carbide filter cake and sodium hydroxide as raw materials, dissolves the silicon carbide filter cake and sodium hydroxide in water respectively, suspends the silicon carbide filter cake into the alkali solution to carry out the silicon removal reaction, and then adds water to carry out the pressure filtration. Until the pH is neutral, a crude wet silicon carbide is obtained.
- the method for purifying the silicon carbide filter cake by alkali washing the steps of the method are as follows: )) mixing the silicon carbide filter cake with water by a weight ratio of 1 and stirring uniformly; mixing sodium hydroxide with water at 1:2, and stirring uniformly;
- the initial reaction temperature is 60 ° C and the reaction temperature is 90 ° C.
- the silicon carbide wet product has a water to mass ratio of 1, and is washed to a pH of 7-8 and a silicon carbide content of 98% or more.
- the beneficial effects of the present invention are as follows: Compared with the prior art, the present invention adopts a titration reaction method to remove the silicon powder alkali reaction, and suspends the silicon carbide suspension into the alkaline water, the reaction temperature is always controlled at 90 ° C, and the gas is uniformly generated. Will not cause boiling state; greatly reduce the amount of alkali and water, alkali and silicon powder 2: 1 feeding, can fully react, save production costs; after the washing alkali using filter press, fast, water saving, can effectively reduce sewage treatment Cost, shorten the production cycle; The purified silicon carbide content of the invention is above 98%.
- the silicon carbide filter cake is washed and purified by a titration method, and the reaction temperature is maintained at 90 ° C, and the alkali and silicon powder are fully reacted; the silicon carbide is washed by pressure filtration to greatly reduce the amount of alkali and water, and shorten Production cycle, reducing environmental pollution.
- the 2000L reaction bottom valve is slowly opened, the silicon carbide filter cake suspension is slowly injected into the 6000L reaction tank, and the silicon powder reacts with the alkali.
- the temperature is raised from 60 ° C to 90 ° C, the 2000 L reaction bottom valve is closed and opened.
- the cooling water of the 6000L reactor was kept at a reaction temperature of 90 ⁇ 2 °C for about 3-4 hours.
- the suspension of the silicon carbide filter cake was completed, and the reaction time in the autoclave was extended for 1 hour.
- the silicon carbide suspension is put into the plate and frame filter press for pressure filtration to obtain 1050kg of crude wet silicon carbide.
- the 1050kg wet silicon carbide crude product is put into 1050kg water and stirred evenly.
- the pressure is filtered again, and the process is repeated 1-2 times until the crude silicon carbide is detected between pH 7-8, and the crude wet silicon carbide is finally obtained as 960kg. %%,
- the silicon carbide content is 98.2% (calculated as dry product), the yield is 94.27% (calculated as pure silicon carbide).
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
提供一种碳化硅滤饼碱洗提纯方法,包括:(1)将碳化硅滤饼与水按重量比以1:1混合并搅拌均匀;将氢氧化钠与水以1:2混合并搅拌均匀;(2)将碳化硅滤饼悬浮液缓慢注入碱水中进行碱反应;(3)将反应后的碳化硅悬浮液按1:1加入水,分别进行3-4次压滤得到碳化硅湿品。经提纯后的碳化硅含量达98%以上。
Description
说 明 书 一种碳化硅滤饼碱洗提纯方法 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, 得到的碳化硅滤饼, 再提纯碳化硅的方法。
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%。 在提纯过程中, 需加入氢氧化钠与硅粉进行反应, 从而去除硅粉, 传统工艺是将碳化硅滤饼投入水中, 再分批加入氢氧化钠固体进行反应, 期 间产生大量的气体, 温度高达 120°C, 沸腾状态, 物料容易从反应釜或者反 应池中喷出, 造成物料损失; 加碱量是硅粉量的几倍, 从而造成生产成本上 升, 后道洗碱水用量大, 污水处理成本高。
发明内容
本发明的目的是提供一种碳化硅滤饼碱洗提纯方法,适合工业规模化生 产。 本发明采用以碳化硅滤饼、 氢氧化钠为原料, 将碳化硅滤饼和氢氧化钠 分别溶在水中, 碳化硅滤饼悬浮液滴入碱溶液中进行除硅反应, 再加水进行 压滤, 直至 pH为中性, 得到湿碳化硅粗品。
本发明的目的是通过采用以下技术方案来实现的:
碳化硅滤饼碱洗提纯方法, 所述方法的步骤如下:
α)将碳化硅滤饼与水按重量比以 1进行混合, 搅拌均匀; 将氢氧化钠 与水以 1 : 2进行混合, 搅拌均匀;
(2 ) 将碳化硅滤饼悬浮液缓慢注入碱水中, 进行碱反应;
(3 )将反应后的碳化硅悬浮液按 1 : 1加入水, 分别进行 3-4次压滤得到碳 化硅湿品。
作为本发明的优选技术方案, 所述初始反应温度为 60°C, 反应温度为 90°C。
作为本发明的优选技术方案, 所述碳化硅湿品与水质量比 1, 清洗至 pH为 7-8, 碳化硅含量 98%以上。
本发明的有益效果是: 相对于现有技术, 本发明采用滴定式反应方法进 行去除硅粉碱反应, 将碳化硅悬浮液滴入碱水中, 反应温度始终控制在 90 °C, 气体均匀产生, 不会造成沸腾状态; 大大减少碱、 水的用量, 碱与硅粉 2: 1投料, 能充分反应, 节约生产成本; 后道洗碱采用压滤机, 快速、省水, 能够有效降低污水处理成本, 缩短生产周期; 本发明经提纯后的碳化硅含量 达 98%以上。
具体实施方式
碳化硅滤饼碱洗提纯的方法,采用滴定式除硅碱反应,保持反应温度 90 °C, 碱和硅粉充分反应; 采用压滤来进行清洗碳化硅, 大大减少碱、 水的用 量, 缩短生产周期, 减少环境污染。
1、 投料配料
在 2000L反应釜中分别依次加入 1000kg水和 1000kg碳化硅滤饼, 开启 搅拌, 直至碳化硅滤饼完全溶在水中, 形成碳化硅滤饼悬浮液。 在 6000L带 夹套的反应罐中加入 300kg氢氧化钠和 600kg水, 期间会发生溶解放热, 水 温约在 45°C, 开启搅拌并开启夹套蒸汽加热, 至水温在 60 ± 2 °C, 关闭蒸汽 加热, 保持搅拌。
2、 除硅碱反应
将 2000L反应釜底阀缓慢打开,碳化硅滤饼悬浮液缓慢注入 6000L反应 釜中, 硅粉与碱进行反应, 温度从 60°C升至 90°C时, 关小 2000L反应釜底 阀, 打开 6000L反应釜的冷却水, 保持釜内反应温度为 90 ± 2 °C, 约 3-4小 时, 碳化硅滤饼悬浮液滴加完毕, 延长釜内反应时间 1小时。
3、 压滤洗碱
6000L反应釜内延长反应完毕后, 加入 2500kg水, 搅拌均匀, 水溶液 pH值约为 12, 将该碳化硅悬浮液打入板框压滤机内进行压滤, 得湿碳化硅 粗品 1050kg,再将该 1050kg湿碳化硅粗品投入 1050kg水中搅拌均匀,再次 压滤, 依次该工序 1-2次, 直至碳化硅粗品检测 pH值 7-8之间, 最终得到 湿碳化硅粗品为 960kg, 经检测水分 20%, 碳化硅含量为 98. 2% (折合干品计 算), 收率 94. 27% (折合纯碳化硅计算)。
Claims
1、 一种碳化硅滤饼碱洗提纯方法, 其特征是所述方法的步骤如下:
(1)将碳化硅滤饼与水按重量比以 1进行混合, 搅拌均匀; 将氢氧化钠 与水以 1: 2进行混合, 搅拌均匀;
(2) 将碳化硅滤饼悬浮液缓慢注入碱水中, 进行碱反应;
(3)将反应后的碳化硅悬浮液按 1: 1加入水, 分别进行 3-4次压滤得到碳 化硅湿品。
2、 根据权利要求 1所述的碳化硅滤饼碱洗提纯方法, 其特征是: 所述 初始反应温度为 60°C, 反应温度为 90°C。
3、 根据权利要求 1所述的碳化硅滤饼碱洗提纯方法, 其特征是: 所述 碳化硅湿品与水质量比 1: 1, 清洗至 pH为 7-8, 碳化硅含量 98%以上。
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CN103241739A (zh) * | 2013-05-16 | 2013-08-14 | 周彬 | 一种碳化硅滤饼碱洗提纯方法 |
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 |
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 |
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CN102031193A (zh) * | 2010-11-02 | 2011-04-27 | 薛荣秀 | 一种从硅片切割废砂浆中回收碳化硅和聚乙二醇切削液的方法 |
CN102060297A (zh) * | 2010-11-26 | 2011-05-18 | 临沭山田研磨材有限公司 | 一种碳化硅微粉和燃料柴油的提取方法 |
CN102746935A (zh) * | 2012-08-02 | 2012-10-24 | 无锡和荣科技有限公司 | 一种硅切割废砂浆回收利用的方法 |
CN103241739A (zh) * | 2013-05-16 | 2013-08-14 | 周彬 | 一种碳化硅滤饼碱洗提纯方法 |
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CN102031193A (zh) * | 2010-11-02 | 2011-04-27 | 薛荣秀 | 一种从硅片切割废砂浆中回收碳化硅和聚乙二醇切削液的方法 |
CN102060297A (zh) * | 2010-11-26 | 2011-05-18 | 临沭山田研磨材有限公司 | 一种碳化硅微粉和燃料柴油的提取方法 |
CN102746935A (zh) * | 2012-08-02 | 2012-10-24 | 无锡和荣科技有限公司 | 一种硅切割废砂浆回收利用的方法 |
CN103241739A (zh) * | 2013-05-16 | 2013-08-14 | 周彬 | 一种碳化硅滤饼碱洗提纯方法 |
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