WO2021026958A1 - Method for preparing white carbon black by means of crystalline silicon diamond wire cut waste - Google Patents
Method for preparing white carbon black by means of crystalline silicon diamond wire cut waste Download PDFInfo
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- WO2021026958A1 WO2021026958A1 PCT/CN2019/101971 CN2019101971W WO2021026958A1 WO 2021026958 A1 WO2021026958 A1 WO 2021026958A1 CN 2019101971 W CN2019101971 W CN 2019101971W WO 2021026958 A1 WO2021026958 A1 WO 2021026958A1
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- C—CHEMISTRY; METALLURGY
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
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- C01—INORGANIC CHEMISTRY
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- the present invention provides a method for preparing white carbon black from the crystalline silicon diamond wire cutting waste.
- the method of the present invention is carried out in the following steps:
- composition of the above-mentioned crystalline silicon diamond wire cutting waste material contains Si ⁇ 97% by mass percentage.
- the lye is sodium hydroxide solution, potassium hydroxide solution, barium hydroxide solution or ammonia; the mass concentration of sodium hydroxide solution, potassium hydroxide solution and barium hydroxide solution is 2-55%, and the mass of ammonia The concentration is 2-25%.
- the amount of lye and the crystalline silicon diamond wire cutting waste is as follows; the molar ratio of Si in the crystalline silicon diamond wire cutting waste to the lye solute is 1: (1-10).
- the inorganic acid solution is hydrochloric acid, sulfuric acid or nitric acid; the mass concentration of sulfuric acid and nitric acid is 1 to 90%, and the mass concentration of hydrochloric acid is 1 to 35%.
- the purity of the above-mentioned white carbon black is ⁇ 99%.
- the method of the present invention has advantages including:
- Fig. 1 is a schematic flow chart of the method for preparing white carbon black by cutting waste with crystalline silicon diamond wire according to the present invention.
- the crystalline silicon diamond wire cutting waste used in the embodiment of the present invention is provided by Henan Xinda New Materials Co., Ltd.
- the drying temperature is 60-140°C and the time is 2-8h.
- the recovery rate of silicon in the embodiment of the present invention is more than 99%.
- the stirring method is mechanical stirring or ultrasonic stirring, and the ultrasonic stirring uses an ultrasonic stirrer.
- composition of crystalline silicon diamond wire cutting waste contains Si ⁇ 97% by mass percentage
- the crystalline silicon diamond wire cutting waste to the lye, stir for 6h at a temperature of 20°C, and then filter to remove the filter residue to obtain the filtrate;
- the lye is sodium hydroxide solution with a mass concentration of 10%;
- the crystalline silicon diamond wire cutting waste The molar ratio of Si to lye solute is 1:4;
- the inorganic acid solution was added dropwise to the filtrate.
- the pH of the mixed solution was 7.0, the reaction was completed; the inorganic acid solution was hydrochloric acid with a mass concentration of 20%;
- the reacted materials are filtered, the obtained solid-phase water is washed until the washing liquid is neutral, and the water is removed by drying to prepare white carbon black with a purity of ⁇ 99%.
- the inorganic acid solution is added dropwise at a temperature of 90°C, and the reaction is completed when the pH value is 8.0; the inorganic acid solution is nitric acid with a mass concentration of 90%.
Abstract
A method for preparing white carbon black by means of crystalline silicon diamond wire cut waste, comprising the following steps: (1) adding crystalline silicon diamond wire cut waste into alkali liquor, stirring under the condition of 20-90°C, and filtering to obtain a filtrate; (2) while stirring, adding an inorganic acid solution dropwise under the condition of 20-90°C, and when the pH value is 6.0-8.0, completing the reaction; and (3) drying after filtering and washing, and preparing the white carbon black. The method can produce high-quality white carbon black at a low cost, and the utilization rate of discarded cut waste is increased.
Description
本发明属于材料技术领域，特别涉及一种用晶体硅金刚线切割废料制备白炭黑的方法。The invention belongs to the technical field of materials, and particularly relates to a method for preparing white carbon black by cutting waste materials with crystalline silicon diamond wire.
近年来，光伏行业迅速发展，为解决能源问题和环境问题做出了巨大贡献；但在光伏行业发展的过程中，也有新的问题出现；生产晶体硅片的方法是将晶体硅棒进行切割，目前主要有两种切割方式：金刚线切割和砂浆切割；由于金刚线切割效率更高、产品精度更高等优势，正逐渐取代砂浆切割成为主要切割方式；而在金刚线切割晶体硅棒的过程中，由于金刚线的直径与所要切割的晶体硅片的厚度相差无几，导致实际生产中有将近50％的原料变为切割废料；切割废料的硅含量非常高且粒度非常小，大量堆积不仅会造成环境污染而且也是一种浪费。In recent years, the photovoltaic industry has developed rapidly and has made great contributions to solving energy and environmental problems. However, in the development of the photovoltaic industry, new problems have also emerged; the method of producing crystalline silicon wafers is to cut crystalline silicon rods. There are currently two main cutting methods: diamond wire cutting and mortar cutting; due to the higher efficiency of diamond wire cutting and higher product accuracy, it is gradually replacing mortar cutting as the main cutting method; and in the process of diamond wire cutting crystalline silicon rods Because the diameter of the diamond wire is almost the same as the thickness of the crystalline silicon wafer to be cut, nearly 50% of the raw materials in actual production become cutting waste; the silicon content of the cutting waste is very high and the particle size is very small, and a large amount of accumulation will not only cause Environmental pollution is also a waste.
白炭黑是一种性能优异的助剂，主要应用于轮胎制造领域、硅橡胶领域、涂料领域等；目前白炭黑的制备方法主要有两种：化学沉淀法和气相法。其中化学沉淀法成本低、对设备要求不高，但是存在产品粒径大或者分布范围宽的问题；气相法制备的白炭黑纯度高、粒径小且分布均匀，但是存在原料价格昂贵、生产流程长、设备要求高、能耗大的问题。Silica is an additive with excellent performance, mainly used in tire manufacturing, silicone rubber, coatings, etc. At present, there are two main methods for preparing white carbon: chemical precipitation method and gas phase method. Among them, the chemical precipitation method has low cost and low equipment requirements, but it has the problem of large product particle size or wide distribution range; the white carbon black prepared by the gas phase method has high purity, small particle size and uniform distribution, but there are expensive raw materials and production Problems with long processes, high equipment requirements and high energy consumption.
发明概述Summary of the invention
问题的解决方案The solution to the problem
针对目前白炭黑制备方法存在的问题，以及晶体硅金刚线切割废料得不到有效利用的问题，本发明提供一种用晶体硅金刚线切割废料制备白炭黑的方法。In view of the problems existing in the current preparation method of white carbon black and the problem that the crystalline silicon diamond wire cutting waste cannot be effectively used, the present invention provides a method for preparing white carbon black from the crystalline silicon diamond wire cutting waste.
本发明的方法按以下步骤进行：The method of the present invention is carried out in the following steps:
1、将晶体硅金刚线切割废料加入到碱液中，在温度20～90℃条件下搅拌1～6h， 然后过滤去除滤渣，获得滤液；1. Add the crystalline silicon diamond wire cutting waste into the lye, stir for 1 to 6 hours at a temperature of 20 to 90°C, and then filter to remove the filter residue to obtain a filtrate;
2、在温度20～90℃和搅拌条件下，向滤液中滴加无机酸溶液，当混合液的pH值为6.0～8.0时，完成反应；2. Under the condition of temperature 20～90℃ and stirring, add the inorganic acid solution dropwise to the filtrate. When the pH value of the mixture is 6.0～8.0, the reaction is completed;
3、将反应后的物料过滤，获得的固相水洗至洗液为中性，烘干去除水分，制成白炭黑。3. Filter the reacted materials, wash the obtained solid phase with water until the lotion is neutral, dry to remove water, and make white carbon black.
上述的晶体硅金刚线切割废料的成分按质量百分比含Si≥97％。The composition of the above-mentioned crystalline silicon diamond wire cutting waste material contains Si≥97% by mass percentage.
上述的步骤1中，碱液为氢氧化钠溶液、氢氧化钾溶液、氢氧化钡溶液或氨水；氢氧化钠溶液、氢氧化钾溶液和氢氧化钡溶液质量浓度2～55％，氨水的质量浓度2～25％。In the above step 1, the lye is sodium hydroxide solution, potassium hydroxide solution, barium hydroxide solution or ammonia; the mass concentration of sodium hydroxide solution, potassium hydroxide solution and barium hydroxide solution is 2-55%, and the mass of ammonia The concentration is 2-25%.
上述的步骤1中，碱液与晶体硅金刚线切割废料的用量按；晶体硅金刚线切割废料中的Si与碱液溶质的摩尔比为1∶(1～10)。In the above step 1, the amount of lye and the crystalline silicon diamond wire cutting waste is as follows; the molar ratio of Si in the crystalline silicon diamond wire cutting waste to the lye solute is 1: (1-10).
上述的步骤2中，无机酸溶液为盐酸、硫酸或硝酸；硫酸和硝酸的质量浓度为1～90％，盐酸的质量浓度为1～35％。In the above step 2, the inorganic acid solution is hydrochloric acid, sulfuric acid or nitric acid; the mass concentration of sulfuric acid and nitric acid is 1 to 90%, and the mass concentration of hydrochloric acid is 1 to 35%.
上述的白炭黑的纯度≥99％。The purity of the above-mentioned white carbon black is ≥99%.
发明的有益效果The beneficial effects of the invention
本发明的方法与现有的技术相比，优点包括：Compared with the existing technology, the method of the present invention has advantages including:
1、使用晶体硅金刚线切割废料制备白炭黑，与现有制备白炭黑的方法相比，原料价格低廉，产品质量相同，可以低成本生产高质量的白炭黑；1. Use crystalline silicon diamond wire to cut waste to prepare white carbon black. Compared with the existing method of preparing white carbon black, the raw material price is low, the product quality is the same, and high-quality white carbon black can be produced at low cost;
2、以晶体硅金刚线切割废料为原料制备白炭黑，提高了废弃切割废料的利用率，有利于废弃物的回收利用。2. Using crystalline silicon diamond wire cutting waste as a raw material to prepare white carbon black, which improves the utilization rate of waste cutting waste and facilitates the recycling of waste.
对附图的简要说明Brief description of the drawings
图1是本发明的用晶体硅金刚线切割废料制备白炭黑的方法流程示意图。Fig. 1 is a schematic flow chart of the method for preparing white carbon black by cutting waste with crystalline silicon diamond wire according to the present invention.
发明实施例Invention embodiment
本发明实施例中采用的晶体硅金刚线切割废料由河南新大新材料有限公司提供 。The crystalline silicon diamond wire cutting waste used in the embodiment of the present invention is provided by Henan Xinda New Materials Co., Ltd.
本发明实施例中烘干温度60～140℃，时间2～8h。In the embodiment of the present invention, the drying temperature is 60-140°C and the time is 2-8h.
本发明实施例中硅的回收率99％以上。The recovery rate of silicon in the embodiment of the present invention is more than 99%.
本发明实施例中搅拌方式为机械搅拌或超声搅拌，其中超声搅拌是采用超声波搅拌器。In the embodiment of the present invention, the stirring method is mechanical stirring or ultrasonic stirring, and the ultrasonic stirring uses an ultrasonic stirrer.
实施例1Example 1
晶体硅金刚线切割废料的成分按质量百分比含Si≥97％；The composition of crystalline silicon diamond wire cutting waste contains Si≥97% by mass percentage;
流程如图1所示；The process is shown in Figure 1;
将晶体硅金刚线切割废料加入到碱液中，在温度20℃条件下搅拌6h，然后过滤去除滤渣，获得滤液；碱液为氢氧化钠溶液，质量浓度10％；晶体硅金刚线切割废料中的Si与碱液溶质的摩尔比为1∶4；Add the crystalline silicon diamond wire cutting waste to the lye, stir for 6h at a temperature of 20℃, and then filter to remove the filter residue to obtain the filtrate; the lye is sodium hydroxide solution with a mass concentration of 10%; the crystalline silicon diamond wire cutting waste The molar ratio of Si to lye solute is 1:4;
在温度20℃和搅拌条件下，向滤液中滴加无机酸溶液，当混合液的pH值为7.0时，完成反应；无机酸溶液为盐酸，质量浓度20％；Under stirring conditions at a temperature of 20°C, the inorganic acid solution was added dropwise to the filtrate. When the pH of the mixed solution was 7.0, the reaction was completed; the inorganic acid solution was hydrochloric acid with a mass concentration of 20%;
将反应后的物料过滤，获得的固相水洗至洗液为中性，烘干去除水分，制成白炭黑，纯度≥99％。The reacted materials are filtered, the obtained solid-phase water is washed until the washing liquid is neutral, and the water is removed by drying to prepare white carbon black with a purity of ≥99%.
实施例2Example 2
方法同实施例1，不同点在于：The method is the same as in Example 1, the difference is:
(1)在温度30℃条件下搅拌5h后过滤；碱液为氢氧化钾溶液，质量浓度55％；晶体硅金刚线切割废料中的Si与碱液溶质的摩尔比为1∶1；(1) Stir at a temperature of 30°C for 5 hours and then filter; the lye is potassium hydroxide solution with a mass concentration of 55%; the molar ratio of Si in the crystalline silicon diamond wire cutting waste to the lye solute is 1:1;
(2)在温度50℃滴加无机酸溶液，pH值为6.0时完成反应；无机酸溶液为硫酸，质量浓度50％。(2) Add an inorganic acid solution dropwise at a temperature of 50°C, and complete the reaction when the pH is 6.0; the inorganic acid solution is sulfuric acid with a mass concentration of 50%.
实施例3Example 3
方法同实施例1，不同点在于：The method is the same as in Example 1, the difference is:
(1)在温度40℃条件下搅拌4.5h后过滤；碱液为氢氧化钡溶液，质量浓度2％；晶体硅金刚线切割废料中的Si与碱液溶质的摩尔比为1∶10；(1) Stir for 4.5 hours at a temperature of 40°C and then filter; the lye is barium hydroxide solution with a mass concentration of 2%; the molar ratio of Si in the crystalline silicon diamond wire cutting waste to the lye solute is 1:10;
(2)在温度90℃滴加无机酸溶液，pH值为8.0时完成反应；无机酸溶液为硝酸，质量浓度90％。(2) The inorganic acid solution is added dropwise at a temperature of 90°C, and the reaction is completed when the pH value is 8.0; the inorganic acid solution is nitric acid with a mass concentration of 90%.
实施例4Example 4
方法同实施例1，不同点在于：The method is the same as in Example 1, the difference is:
(1)在温度60℃条件下搅拌3h后过滤；碱液为氨水，质量浓度25％；晶体硅金刚线切割废料中的Si与碱液溶质的摩尔比为1∶6；(1) Stir at a temperature of 60°C for 3 hours and then filter; the lye is ammonia water with a mass concentration of 25%; the molar ratio of Si in the crystalline silicon diamond wire cutting waste to the lye solute is 1:6;
(2)在温度20～90℃滴加无机酸溶液，pH值为6.5时完成反应；无机酸溶液为盐酸，质量浓度35％。(2) Add the inorganic acid solution dropwise at a temperature of 20-90°C, and complete the reaction when the pH is 6.5; the inorganic acid solution is hydrochloric acid with a mass concentration of 35%.
实施例5Example 5
方法同实施例1，不同点在于：The method is the same as in Example 1, the difference is:
(1)在温度90℃条件下搅拌1h后过滤；碱液为氨水，质量浓度2％；晶体硅金刚线切割废料中的Si与碱液溶质的摩尔比为1∶3；(1) Stir at a temperature of 90°C for 1 hour and then filter; the lye is ammonia water with a mass concentration of 2%; the molar ratio of Si in the crystalline silicon diamond wire cutting waste to the lye solute is 1:3;
(2)在温度20～90℃滴加无机酸溶液，pH值为7.5时完成反应；无机酸溶液为盐酸、硫酸或硝酸；硫酸和硝酸的质量浓度为1～90％，盐酸的浓度为1～35％。(2) Add mineral acid solution dropwise at a temperature of 20～90℃, and complete the reaction when the pH is 7.5; mineral acid solution is hydrochloric acid, sulfuric acid or nitric acid; the mass concentration of sulfuric acid and nitric acid is 1 to 90%, and the concentration of hydrochloric acid is 1 ~ 35%.
实施例6Example 6
方法同实施例1，不同点在于：The method is the same as in Example 1, the difference is:
(1)在温度80℃条件下搅拌1.5h后过滤；碱液为氢氧化钾溶液，质量浓度2％；晶体硅金刚线切割废料中的Si与碱液溶质的摩尔比为1∶8；(1) Stir at a temperature of 80°C for 1.5 hours and then filter; the lye is potassium hydroxide solution with a mass concentration of 2%; the molar ratio of Si in the crystalline silicon diamond wire cutting waste to the lye solute is 1:8;
(2)在温度20～90℃滴加无机酸溶液，pH值为7.0时完成反应；无机酸溶液为盐酸，质量浓度1％。(2) Add the inorganic acid solution dropwise at a temperature of 20-90°C, and complete the reaction when the pH is 7.0; the inorganic acid solution is hydrochloric acid with a mass concentration of 1%.
Claims (6)
- 一种用晶体硅金刚线切割废料制备白炭黑的方法，其特征在于按以下步骤进行：A method for preparing white carbon black by cutting waste with crystalline silicon diamond wire, which is characterized in that it is carried out in the following steps:(1)将晶体硅金刚线切割废料加入到碱液中，在温度20～90℃条件下搅拌1～6h，然后过滤去除滤渣，获得滤液；(1) Add the crystalline silicon diamond wire cutting waste into the lye, stir for 1 to 6 hours at a temperature of 20 to 90°C, and then filter to remove the filter residue to obtain a filtrate;(2)在温度20～90℃和搅拌条件下，向滤液中滴加无机酸溶液，当混合液的pH值为6.0～8.0时，完成反应；(2) Under the condition of temperature 20～90℃ and stirring, add the inorganic acid solution dropwise to the filtrate. When the pH value of the mixture is 6.0～8.0, the reaction is completed;(3)将反应后的物料过滤，获得的固相水洗至洗液为中性，烘干去除水分，制成白炭黑。(3) Filter the reacted materials, wash the obtained solid phase with water until the washing liquid is neutral, and dry to remove water to prepare white carbon black.
- 根据权利要求1所述的一种用晶体硅金刚线切割废料制备白炭黑的方法，其特征在于所述的晶体硅金刚线切割废料的成分按质量百分比含Si≥97％。The method for preparing white carbon black from crystalline silicon diamond wire cutting waste according to claim 1, wherein the composition of the crystalline silicon diamond wire cutting waste contains Si≥97% by mass percentage.
- 根据权利要求1所述的一种用晶体硅金刚线切割废料制备白炭黑的方法，其特征在于所述的碱液为氢氧化钠溶液、氢氧化钾溶液、氢氧化钡溶液或氨水；氢氧化钠溶液、氢氧化钾溶液和氢氧化钡溶液质量浓度2～55％，氨水的质量浓度2～25％。The method for preparing white carbon black by cutting waste from crystalline silicon diamond wire according to claim 1, wherein the lye is sodium hydroxide solution, potassium hydroxide solution, barium hydroxide solution or ammonia; hydrogen The mass concentration of sodium oxide solution, potassium hydroxide solution and barium hydroxide solution is 2 to 55%, and the mass concentration of ammonia water is 2 to 25%.
- 根据权利要求1所述的一种用晶体硅金刚线切割废料制备白炭黑的方法，其特征在于步骤(1)中，碱液与晶体硅金刚线切割废料的用量按；晶体硅金刚线切割废料中的Si与碱液溶质的摩尔比为1∶(1～10)。The method for preparing white carbon black by using crystalline silicon diamond wire cutting waste according to claim 1, wherein in step (1), the amount of lye and crystalline silicon diamond wire cutting waste is as follows; crystalline silicon diamond wire cutting The molar ratio of Si in the waste to the lye solute is 1: (1-10).
- 根据权利要求1所述的一种用晶体硅金刚线切割废料制备白炭黑的方法，其特征在于所述的无机酸溶液为盐酸、硫酸或硝酸；硫酸和硝酸的质量浓度为1～90％，盐酸的质量浓度为1～35％。The method for preparing white carbon black by cutting waste from crystalline silicon diamond wire according to claim 1, wherein the inorganic acid solution is hydrochloric acid, sulfuric acid or nitric acid; the mass concentration of sulfuric acid and nitric acid is 1 to 90% , The mass concentration of hydrochloric acid is 1 to 35%.
- 根据权利要求1所述的一种用晶体硅金刚线切割废料制备白炭黑的方法，其特征在于所述的白炭黑的纯度≥99％。The method for preparing white carbon black by cutting waste from crystalline silicon diamond wire according to claim 1, wherein the purity of the white carbon black is ≥99%.
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