CN1562742A - Method for preparing submicro and nano silicon dioxide in spherical shape - Google Patents
Method for preparing submicro and nano silicon dioxide in spherical shape Download PDFInfo
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- CN1562742A CN1562742A CN 200410012854 CN200410012854A CN1562742A CN 1562742 A CN1562742 A CN 1562742A CN 200410012854 CN200410012854 CN 200410012854 CN 200410012854 A CN200410012854 A CN 200410012854A CN 1562742 A CN1562742 A CN 1562742A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 16
- 235000012239 silicon dioxide Nutrition 0.000 title claims abstract description 7
- 239000005543 nano-size silicon particle Substances 0.000 title 1
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 25
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- 230000032683 aging Effects 0.000 claims abstract description 6
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000004111 Potassium silicate Substances 0.000 claims abstract description 5
- 239000002245 particle Substances 0.000 claims abstract description 5
- 229910052913 potassium silicate Inorganic materials 0.000 claims abstract description 5
- 235000019353 potassium silicate Nutrition 0.000 claims abstract description 5
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 claims abstract description 5
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 4
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 4
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims abstract description 3
- 239000000463 material Substances 0.000 claims abstract description 3
- 238000004381 surface treatment Methods 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 7
- 230000003068 static effect Effects 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 230000008676 import Effects 0.000 claims 1
- 230000001105 regulatory effect Effects 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000004806 packaging method and process Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 6
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 238000000593 microemulsion method Methods 0.000 description 2
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009841 combustion method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002431 foraging effect Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
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- Silicon Compounds (AREA)
Abstract
本发明公开了一种制备亚微米和纳米球形二氧化硅的方法，将含二氧化硅1～20wt％的硅酸钾、硅酸钠或碱性硅溶胶和1～20wt％的硫酸分别按1～300L/min流量连续导入反应容器，搅拌让物料保持紊流循环1～100min，静置陈化后分离；用25～100℃的去离子水洗涤产物至pH 5～7，烘干，即得粒度5μm～10nm亚微米和纳米球形二氧化硅。本发明的制备方法工艺过程简单，能耗低；产品比表面积可以通过加热温度调控，产品的纯度高，流动性好，易分散，粒度在5μm～10nm间调控，适合于超大规模集成电路的封装料制备，也可以用于机械、电子、日用化工、生物医药等领域。The invention discloses a method for preparing submicron and nano-spherical silicon dioxide. Potassium silicate, sodium silicate or alkaline silica sol containing 1 to 20 wt % of silicon dioxide and 1 to 20 wt % of sulfuric acid are respectively pressed by 1 The flow rate of ~300L/min is continuously introduced into the reaction vessel, stirred to keep the material in turbulent flow for 1~100min, separated after standing and aging; the product is washed with deionized water at 25~100℃ to pH 5~7, and dried to obtain Submicron and nano-spherical silica with a particle size of 5 μm to 10 nm. The preparation method of the present invention has simple technological process and low energy consumption; the specific surface area of the product can be regulated by heating temperature, the product has high purity, good fluidity, and is easy to disperse; the particle size can be regulated between 5 μm and 10 nm; it is suitable for the packaging of VLSI It can also be used in machinery, electronics, daily chemical industry, biomedicine and other fields.
Description
技术领域technical field
本发明涉及一种亚微米和纳米球形二氧化硅的制备方法，属于无机新材料技术领域。The invention relates to a method for preparing submicron and nano-spherical silicon dioxide, belonging to the technical field of new inorganic materials.
背景技术Background technique
亚微米和纳米球形二氧化硅可用于超大规模集成电路的封装料制备，也可以用于机械、电子、日用化工、生物医药等领域。Sub-micron and nano-spherical silica can be used in the preparation of packaging materials for VLSI, and can also be used in machinery, electronics, daily chemical industry, biomedicine and other fields.
根据文献报道，现有亚微米和纳米球形二氧化硅的方法主要有以下几种：1、由硅酸钾(钠)与酸反应得到硅溶胶后再高温喷射制备亚微米和纳米球形二氧化硅；2、有机硅水解制备亚微米和纳米球形二氧化硅；3、硅石在高温下还原成一氧化硅后再汽化氧化形成亚微米和纳米球形二氧化硅；4、二氧化硅块直接高温汽化-冷凝制备亚微米和纳米球形二氧化硅；5、有机硅喷雾燃烧制备亚微米和纳米球形二氧化硅；6、微乳液法制备亚微米和纳米球形二氧化硅。由于上述方法采用高温喷射、有机硅水解、高温下汽化、喷雾燃烧或微乳液法等，其制备复杂、能耗高。According to literature reports, the existing methods of submicron and nano-spherical silica mainly contain the following: 1. Prepare sub-micron and nano-spherical silica by spraying at high temperature after obtaining silica sol by reacting potassium silicate (sodium) with acid ; 2. Organic silicon hydrolysis to prepare submicron and nano-spherical silica; 3. Silica is reduced to silicon monoxide at high temperature and then vaporized and oxidized to form sub-micron and nano-spherical silica; 4. Silica blocks are directly vaporized at high temperature- Preparation of submicron and nano-spherical silica by condensation; 5. Preparation of sub-micron and nano-spherical silica by organosilicon spray combustion; 6. Preparation of sub-micron and nano-spherical silica by microemulsion method. Since the above method adopts high-temperature injection, organosilicon hydrolysis, vaporization at high temperature, spray combustion or microemulsion method, etc., its preparation is complicated and energy-consuming.
发明内容Contents of the invention
为了克服现有技术的不足，本发明提供了一种亚微米和纳米球形二氧化硅的制备方法。该方法条件温和，工艺过程简单，所得产品流动性好、分散性好、比表面积可控。In order to overcome the deficiencies of the prior art, the invention provides a method for preparing submicron and nano-spherical silicon dioxide. The method has mild conditions, simple process, and the obtained product has good fluidity, good dispersibility and controllable specific surface area.
为实现本发明的目的所采取的技术措施是：The technical measures taken for realizing the purpose of the present invention are:
一种制备亚微米和纳米球形二氧化硅的方法，一种制备亚微米和纳米球形二氧化硅的方法，将含二氧化硅1～20wt％的硅酸钾、硅酸钠或碱性硅溶胶和1～20wt％的硫酸分别按1～300L/min流量连续导入反应容器，搅拌让物料保持紊流循环1～100min，静置陈化后分离；用25～100℃的去离子水洗涤产物至pH5～7，烘干，即得粒度5μm～10nm亚微米和纳米球形二氧化硅。A method for preparing submicron and nano-spherical silica, a method for preparing sub-micron and nano-spherical silica, comprising potassium silicate, sodium silicate or alkaline silica sol containing 1 to 20 wt% of silica and 1-20wt% sulfuric acid were continuously introduced into the reaction vessel at a flow rate of 1-300L/min, stirred to keep the material in turbulent circulation for 1-100min, separated after standing and aging; the product was washed with deionized water at 25-100°C until pH 5-7, drying to obtain sub-micron and nano-spherical silica with a particle size of 5 μm-10 nm.
根据本发明的技术方案，静置陈化时间10～600min。According to the technical solution of the present invention, the static aging time is 10 to 600 minutes.
根据本发明的技术方案，烘干温度为25至500℃，干燥时间1～10小时。According to the technical solution of the present invention, the drying temperature is 25 to 500° C., and the drying time is 1 to 10 hours.
本发明可根据需要在烘干后进行表面处理，包括加热表面处理和(或)化学表面处理。其中加热表面处理温度范围500～1200℃；化学表面处理为常规干法或湿法表面处理。In the present invention, surface treatment may be carried out after drying as required, including heating surface treatment and (or) chemical surface treatment. The heating surface treatment temperature ranges from 500 to 1200°C; the chemical surface treatment is conventional dry or wet surface treatment.
与现有技术相比较，采用本发明的技术方案所达到的有益效果：Compared with the prior art, the beneficial effects achieved by adopting the technical solution of the present invention are as follows:
本发明的制备方法工艺过程简单，能耗低；产品比表面积可以通过加热温度调控，产品的纯度高，流动性好，易分散，粒度在5μm～10nm间调控，适合于超大规模集成电路的封装料制备，也可以用于机械、电子、日用化工、生物医药等领域。The preparation method of the present invention has simple technological process and low energy consumption; the specific surface area of the product can be regulated by heating temperature, the product has high purity, good fluidity, and is easy to disperse; the particle size can be regulated between 5 μm and 10 nm; it is suitable for the packaging of VLSI It can also be used in machinery, electronics, daily chemical industry, biomedicine and other fields.
具体实施方式Detailed ways
实例1：Example 1:
分别量取1000mL 1.2g/mL硅酸钠和500mL 20％的硫酸溶液，分别以1mL/min和0.5mL/min的流量导入不锈钢容器，并搅拌紊流循环60min后静置陈化时间120min。过滤，用50℃去离子水洗到pH5～7，120℃下干燥2小时，再经过1180度处理得到1微米的球形二氧化硅。Measure 1000mL of 1.2g/mL sodium silicate and 500mL of 20% sulfuric acid solution respectively, and introduce them into stainless steel containers at flow rates of 1mL/min and 0.5mL/min respectively, stir and circulate for 60min in turbulent flow, and then let it stand for 120min for aging. Filter, wash with 50°C deionized water to pH 5-7, dry at 120°C for 2 hours, and then process at 1180°C to obtain 1 micron spherical silica.
实例2：Example 2:
分别量取1000mL 1.1g/mL碱性硅溶胶和20mL 10％的硫酸溶液，分别以50mL/min和1mL/min的流量导入反应器中，紊流循环90min静置陈化时间240min。过滤，用70℃去离子水洗涤到pH5～7，60℃下干燥8小时，再经过1200度处理得到70纳米的球形二氧化硅。Measure 1000mL of 1.1g/mL alkaline silica sol and 20mL of 10% sulfuric acid solution respectively, and introduce them into the reactor at flow rates of 50mL/min and 1mL/min respectively, turbulent flow circulation for 90min and standing aging time for 240min. Filter, wash with 70°C deionized water to pH 5-7, dry at 60°C for 8 hours, and then process at 1200°C to obtain 70nm spherical silica.
实例3：Example 3:
分别量取1000mL 1.1g/mL硅酸钾和500mL 5％的硫酸溶液，分别以1mL/min和0.5mL/min的流量导入反应器中，紊流循环100min静置陈化时间350min。过滤，用30℃去离子水洗涤到pH5～7，200℃下干燥1.5小时，再经过常规常规干法或湿法表面处理得到50纳米的球形二氧化硅。Measure 1000mL of 1.1g/mL potassium silicate and 500mL of 5% sulfuric acid solution respectively, and introduce them into the reactor at the flow rates of 1mL/min and 0.5mL/min respectively, and let the turbulent flow circulate for 100min to stand for 350min. Filter, wash with deionized water at 30°C to pH 5-7, dry at 200°C for 1.5 hours, and then undergo conventional dry or wet surface treatment to obtain 50nm spherical silica.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410012854 CN1273381C (en) | 2004-03-18 | 2004-03-18 | Method for preparing submicro and nano silicon dioxide in spherical shape |
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|---|---|---|---|
| CN 200410012854 CN1273381C (en) | 2004-03-18 | 2004-03-18 | Method for preparing submicro and nano silicon dioxide in spherical shape |
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| CN1562742A true CN1562742A (en) | 2005-01-12 |
| CN1273381C CN1273381C (en) | 2006-09-06 |
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| CN 200410012854 Expired - Fee Related CN1273381C (en) | 2004-03-18 | 2004-03-18 | Method for preparing submicro and nano silicon dioxide in spherical shape |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100447081C (en) * | 2005-09-15 | 2008-12-31 | 成都理工大学 | Method of preparing spherical nanometer SiO2 using powder quartz by chemical precipitation method |
| TWI848506B (en) * | 2022-10-18 | 2024-07-11 | 大陸商江蘇聯瑞新材料股份有限公司 | Method for preparing nano- and submicron spherical oxide fillers |
-
2004
- 2004-03-18 CN CN 200410012854 patent/CN1273381C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100447081C (en) * | 2005-09-15 | 2008-12-31 | 成都理工大学 | Method of preparing spherical nanometer SiO2 using powder quartz by chemical precipitation method |
| TWI848506B (en) * | 2022-10-18 | 2024-07-11 | 大陸商江蘇聯瑞新材料股份有限公司 | Method for preparing nano- and submicron spherical oxide fillers |
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| Publication number | Publication date |
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| CN1273381C (en) | 2006-09-06 |
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