WO2014005272A1 - Silicon dioxide powder material and preparation process therefor - Google Patents
Silicon dioxide powder material and preparation process therefor Download PDFInfo
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- WO2014005272A1 WO2014005272A1 PCT/CN2012/078079 CN2012078079W WO2014005272A1 WO 2014005272 A1 WO2014005272 A1 WO 2014005272A1 CN 2012078079 W CN2012078079 W CN 2012078079W WO 2014005272 A1 WO2014005272 A1 WO 2014005272A1
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- powder material
- silica powder
- organic substance
- silicon dioxide
- dioxide powder
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
Definitions
- the present invention relates to a novel material and a preparation method thereof, and in particular to a novel silica powder material and a preparation method thereof.
- Background technique :
- a new type of silica powder material soft silicon, English name si liesoft, is a silica powder material with a particle size in the range of 0.1 to 30 microns. It can be widely used in machinery, household chemicals, and biology. In the fields of medicine, construction, aerospace, agriculture, etc., it also exhibits singular characteristics in terms of sound, light, electricity, magnetism and thermodynamics. It can also be widely used in microelectronics, information materials, paints, rubber, plastics, crops. Seed treatment agents, polishing agents, LED light diffusers, advanced refractories and papermaking.
- the technical problem to be solved by the present invention is to provide a novel silica powder material having a particle diameter in the range of 0.1 to 30 ⁇ m and a preparation method thereof.
- the concentration of the silica sol is from 1% to 30%, and the particle size of the silica in the silica sol is from 3 to 80 nm.
- the hydrolyzable organic material is a hydrolyzable silicon germanium.
- the new silica powder having a particle size of 0.1 to 30 ⁇ m is prepared by the reaction of the mixture.
- the reaction is carried out at a temperature of 0.1 to 30 ⁇ m. Material.
- the mass ratio of the hydrolyzable organic substance to the silica sol is from 1% to 25%.
- silica powder materials of different particle sizes can be prepared.
- the hydrolyzable organic material is a hydrolyzable silicon germanium.
- the novel silica powder material prepared by the invention has a particle diameter of 0.1 to 30 micrometers and has wide application fields; and the production process is simple, the production equipment used is small, the operation is simple, the preparation cycle end, the manufacturing cost is low, and the production efficiency High; By adjusting the content of hydrolyzable organic matter, it is possible to control the preparation of silica powder materials of different particle sizes.
- FIG. 1 is a SEM photograph of a silica powder material having a particle diameter of 1 ⁇ m prepared according to the present invention
- FIG. 2 is a SEM photograph of a silica powder material having a particle diameter of 3 ⁇ m prepared according to the present invention
- FIG. 4 is a SEM photograph of a silica powder material having a particle diameter of 10 ⁇ m prepared according to the present invention
- Fig. 6 is a schematic view showing the distribution of pore diameter and pore volume of the silica powder material prepared by the present invention.
- a novel method for preparing a silica powder material comprising the following steps:
- the new silica powder material having a particle diameter of 0.1 to 30 ⁇ m is prepared by mixing 10 ml of aminosilicone with 100 ml of silica sol and stirring for 5 hours.
- a novel method for preparing a silica powder material comprising the following steps:
- the new silica powder material having a particle size of 0.1 to 30 ⁇ m is prepared by mixing 10 ml of trimethoxysilane with 120 ml of a silica sol, and stirring for 8 hours.
- a novel method for preparing a silica powder material comprising the following steps:
- the raw material for preparing the novel silica powder material may also be Y-aminopropyltriethoxysilane, Y-aminopropyltrimethoxysilane, Y-(2,3 epoxypropoxy)propyl Trimethoxysilane, Y-methacryloxypropyltrimethoxysilane, Y-mercaptopropyltriethoxysilane, Y-mercaptopropyltrimethoxysilane, ⁇ - ⁇ - (aminoethyl) aminopropylmethyldimethoxysilane, ⁇ -aminopropylmethyldimethoxysilane, ⁇ -aminopropylmethyldiethoxysilane, ⁇ - ⁇ - ( Aminoethyl) aminopropyltriethoxysilane, ⁇ - ⁇ -(aminoethyl)aminopropyltrimethoxysilane, vinyltriethoxysilane, vinyltrimethoxys
Abstract
Provided are a silicon dioxide powder material and a preparation process therefor. The silicon dioxide powder material is a silicon dioxide powder material having a particle size of 0.1-30 microns produced by the aggregation acceleration of a hydrolysable organic substance, with a silica sol as a raw material. The preparation process is as follows: mixing the hydrolysable organic substance with the silica sol in a ratio at normal temperature, reacting for 1-48 hours under the conditions of stirring, and filter-pressing and dewatering after completion of the reaction. The silicon dioxide powder material is widely applicable, simple in production processing, and low in production costs; silicon dioxide powder materials with different particle sizes can be prepared by adjusting the content of the hydrolysable organic substance.
Description
一种二氧化硅粉体材料及其制备方法 技术领域- 本发明涉及一种新材料及其制备方法， 尤其涉及新型二氧化硅粉体材料 及其制备方法。 背景技术： TECHNICAL FIELD The present invention relates to a novel material and a preparation method thereof, and in particular to a novel silica powder material and a preparation method thereof. Background technique:
新型二氧化硅粉体材料——软硅， 英文名称 si liesoft,是一种粒径在 0. 1〜30微米范围内的二氧化硅粉体材料， 可广泛应用于机械、 日用化工、 生 物医药、 建筑业、 航空航天业、 农业等领域， 在声、 光、 电、 磁及热力学等 方面也呈现出奇异的特性， 亦可广泛用于微电子、 信息材料、 涂料、 橡胶、 塑料、 农作物种子处理剂、 抛光剂、 LED光扩散剂、 高级耐火材料及造纸等方 面。 A new type of silica powder material, soft silicon, English name si liesoft, is a silica powder material with a particle size in the range of 0.1 to 30 microns. It can be widely used in machinery, household chemicals, and biology. In the fields of medicine, construction, aerospace, agriculture, etc., it also exhibits singular characteristics in terms of sound, light, electricity, magnetism and thermodynamics. It can also be widely used in microelectronics, information materials, paints, rubber, plastics, crops. Seed treatment agents, polishing agents, LED light diffusers, advanced refractories and papermaking.
现有技术中制备二氧化硅粉体的方法有很多， 但都没有制备粒径在 0. 1〜 30微米范围内的二氧化硅粉体材料。 发明内容： There are many methods for preparing the silica powder in the prior art, but none of the silica powder materials having a particle diameter in the range of 0.1 to 30 μm is prepared. Summary of the invention:
本发明所要解决的技术问题在于提供一种粒径在 0. 1〜30微米范围内的 新型二氧化硅粉体材料及其制备方法。 The technical problem to be solved by the present invention is to provide a novel silica powder material having a particle diameter in the range of 0.1 to 30 μm and a preparation method thereof.
本发明所要解决的技术问题采用以下技术方案来实现： The technical problem to be solved by the present invention is implemented by the following technical solutions:
一种新型二氧化硅粉体材料， 其特征在于： 所述新型二氧化硅粉体材料 是以硅溶胶为原料， 通过可水解有机物的团聚促进作用而生成的粒径在 0. 1〜 30微米的二氧化硅粉体材料。 1〜 30微米。 The particle size of the particle size of 0. 1~ 30 microns Silica powder material.
所述硅溶胶浓度为 1 %〜30 %， 硅溶胶中二氧化硅的粒径为 3〜80纳米。 所述可水解有机物为可水解硅垸。 The concentration of the silica sol is from 1% to 30%, and the particle size of the silica in the silica sol is from 3 to 80 nm. The hydrolyzable organic material is a hydrolyzable silicon germanium.
常温下， 可水解有机物与硅溶胶按比例混合， 在搅拌条件下反应 1〜48小 时， 反应完成后压滤脱水， 即制备出粒径在 0. 1〜30微米的新型二氧化硅粉体
材料。 The new silica powder having a particle size of 0.1 to 30 μm is prepared by the reaction of the mixture. The reaction is carried out at a temperature of 0.1 to 30 μm. Material.
所述可水解有机物与硅溶胶混合的质量比为 1 %〜25 %。 The mass ratio of the hydrolyzable organic substance to the silica sol is from 1% to 25%.
通过调节可水解有机物的含量， 可制备出不同粒径的二氧化硅粉体材料。 所述可水解有机物为可水解硅垸。 By adjusting the content of hydrolyzable organic matter, silica powder materials of different particle sizes can be prepared. The hydrolyzable organic material is a hydrolyzable silicon germanium.
本发明制备的新型二氧化硅粉体材料， 粒径在 0. 1〜30微米， 应用领域广 泛； 并且生产工艺简单， 使用的生产设备少， 操作简便， 制备周期端， 制造 成本低， 生产效率高； 通过调节可水解有机物的含量， 可控制制备出不同粒 径的二氧化硅粉体材料。 附图说明： The novel silica powder material prepared by the invention has a particle diameter of 0.1 to 30 micrometers and has wide application fields; and the production process is simple, the production equipment used is small, the operation is simple, the preparation cycle end, the manufacturing cost is low, and the production efficiency High; By adjusting the content of hydrolyzable organic matter, it is possible to control the preparation of silica powder materials of different particle sizes. BRIEF DESCRIPTION OF THE DRAWINGS:
图 1为本发明制备的粒径为 1微米的二氧化硅粉体材料的 SEM照片； 图 2为本发明制备的粒径为 3微米的二氧化硅粉体材料的 SEM照片； 图 3为本发明制备的粒径为 5微米的二氧化硅粉体材料的 SEM照片； 图 4为本发明制备的粒径为 10微米的二氧化硅粉体材料的 SEM照片； 图 5为本发明制备的粒径为 20微米的二氧化硅粉体材料的 SEM照片； 图 6为本发明制备的二氧化硅粉体材料孔径与孔体积的分布示意图。 具体实施方式- 为了使本发明实现的技术手段、 创作特征、 达成目的与功效易于明白了 解， 下面结合具体实施例， 进一步阐述本发明。 1 is a SEM photograph of a silica powder material having a particle diameter of 1 μm prepared according to the present invention; FIG. 2 is a SEM photograph of a silica powder material having a particle diameter of 3 μm prepared according to the present invention; SEM photograph of a silica powder material having a particle diameter of 5 μm prepared by the invention; FIG. 4 is a SEM photograph of a silica powder material having a particle diameter of 10 μm prepared according to the present invention; SEM photograph of a silica powder material having a diameter of 20 μm; Fig. 6 is a schematic view showing the distribution of pore diameter and pore volume of the silica powder material prepared by the present invention. BEST MODE FOR CARRYING OUT THE INVENTION - In order to make the technical means, the authoring features, the achievement of the object and the effect of the present invention easy to understand, the present invention will be further described below in conjunction with specific embodiments.
实施例一 Embodiment 1
一种新型二氧化硅粉体材料的制备方法， 包括以下步骤： A novel method for preparing a silica powder material, comprising the following steps:
常温下， 将 10ml氨基硅垸与 100ml硅溶胶混合， 搅拌 5小时后， 反应完 成后压滤脱水， 即制备出粒径在 0. 1〜30微米的新型二氧化硅粉体材料。 The new silica powder material having a particle diameter of 0.1 to 30 μm is prepared by mixing 10 ml of aminosilicone with 100 ml of silica sol and stirring for 5 hours.
实施例二 Embodiment 2
一种新型二氧化硅粉体材料的制备方法， 包括以下步骤： A novel method for preparing a silica powder material, comprising the following steps:
常温下， 将 10ml三甲氧基硅垸与 120ml硅溶胶混合， 搅拌 8小时后， 反 应完成后压滤脱水， 即制备出粒径在 0. 1〜30微米的新型二氧化硅粉体材料。
一种新型二氧化硅粉体材料的制备方法， 包括以下步骤： The new silica powder material having a particle size of 0.1 to 30 μm is prepared by mixing 10 ml of trimethoxysilane with 120 ml of a silica sol, and stirring for 8 hours. A novel method for preparing a silica powder material, comprising the following steps:
常温下， 将 10ml四乙氧基硅垸与 150ml硅溶胶混合， 搅拌 6小时后， 反 应完成后压滤脱水， 即制备出粒径在 0.1〜30微米的新型二氧化硅粉体材料。 At room temperature, 10 ml of tetraethoxysilane was mixed with 150 ml of silica sol, and after stirring for 6 hours, the reaction was completed and subjected to pressure filtration and dehydration to prepare a novel silica powder material having a particle diameter of 0.1 to 30 μm.
用于制备新型二氧化硅粉体材料的原料还可选用 Y -氨丙基三乙氧基硅 垸、 Y-氨丙基三甲氧基硅垸、 Y- (2, 3环氧丙氧） 丙基三甲氧基硅垸、 Y- 甲基丙烯酰氧基丙基三甲氧基硅垸、 Y-巯丙基三乙氧基硅垸、 Y-巯丙基三 甲氧基硅垸、 Ν-β - (氨乙基） 氨丙基甲基二甲氧基硅垸、 Υ-氨丙基甲 基二甲氧基硅垸、 Υ-氨丙基甲基二乙氧基硅垸、 Ν-β - (氨乙基） 氨丙 基三乙氧基硅垸、 Ν-β - (氨乙基） 氨丙基三甲氧基硅垸、 乙烯基三乙氧 基硅垸、 乙烯基三甲氧基硅垸、 R-三乙氧基硅垸、 R-三甲氧基硅垸、 苯氨甲 基三乙氧基硅垸、 双- ( Υ-三乙氧基硅丙基） -四硫化物或 Ν-苯基 -3-氨丙基 三甲氧基硅垸等物质。 The raw material for preparing the novel silica powder material may also be Y-aminopropyltriethoxysilane, Y-aminopropyltrimethoxysilane, Y-(2,3 epoxypropoxy)propyl Trimethoxysilane, Y-methacryloxypropyltrimethoxysilane, Y-mercaptopropyltriethoxysilane, Y-mercaptopropyltrimethoxysilane, Ν-β- (aminoethyl) aminopropylmethyldimethoxysilane, Υ-aminopropylmethyldimethoxysilane, Υ-aminopropylmethyldiethoxysilane, Ν-β- ( Aminoethyl) aminopropyltriethoxysilane, Ν-β-(aminoethyl)aminopropyltrimethoxysilane, vinyltriethoxysilane, vinyltrimethoxysilane, R -triethoxysilane, R-trimethoxysilane, benzylaminotriethoxysilane, bis-(antimony-triethoxysilylpropyl)-tetrasulfide or fluorene-phenyl- 3-aminopropyltrimethoxysilane and the like.
以上显示和描述了本发明的基本原理和主要特征和本发明的优点。 本行 业的技术人员应该了解， 本发明不受上述实施例的限制， 上述实施例和说明 书中描述的只是说明本发明的原理， 在不脱离本发明精神和范围的前提下， 本发明还会有各种变化和改进， 这些变化和改进都落入要求保护的本发明范 围内。 本发明要求保护范围由所附的权利要求书及其等效物界定。
The basic principles and main features of the present invention and the advantages of the present invention are shown and described above. It should be understood by those skilled in the art that the present invention is not limited by the foregoing embodiments, and that the present invention is only described in the foregoing embodiments and the description of the present invention, without departing from the spirit and scope of the invention. Various changes and modifications are intended to fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and their equivalents.
Claims
1.一种新型二氧化硅粉体材料， 其特征在于： 所述新型二氧化硅粉体材 料是以硅溶胶为原料， 通过可水解有机物的团聚促进作用而生成的粒径在 A novel silica powder material characterized in that: the novel silica powder material is a silica sol as a raw material, and a particle size generated by agglomeration promoting action of a hydrolyzable organic substance is
0. 1〜30微米的二氧化硅粉体材料。 0. 1~30 micron silica powder material.
2.根据权利要求 1所述的新型二氧化硅粉体材料， 其特征在于： 所述硅溶 胶浓度为 1 %〜30 %， 硅溶胶中二氧化硅的粒径为 3〜80纳米。 The novel silica powder material according to claim 1, wherein the silica sol has a concentration of from 1% to 30%, and the silica sol has a particle diameter of from 3 to 80 nm.
3.根据权利要求 1所述的新型二氧化硅粉体材料， 其特征在于： 所述可水 解有机物为可水解硅垸。 The novel silica powder material according to claim 1, wherein the hydrolyzable organic substance is hydrolyzable silicon germanium.
4.根据权利要求 1所述的新型二氧化硅粉体材料的制备方法， 其特征在 于： 常温下， 可水解有机物与硅溶胶按比例混合， 在搅拌条件下反应 1〜48小 时， 反应完成后压滤脱水， 即制备出粒径在 0. 1〜30微米的新型二氧化硅粉体 材料。 The method for preparing a novel silica powder material according to claim 1, characterized in that: at room temperature, the hydrolyzable organic substance is mixed with the silica sol in a ratio, and reacted under stirring for 1 to 48 hours, after completion of the reaction. The novel silica powder material having a particle diameter of 0.1 to 30 μm is prepared by a pressure filtration.
5.根据权利要求 4所述的新型二氧化硅粉体材料的制备方法， 其特征在 于： 所述可水解有机物与硅溶胶混合的质量比为 1 %〜25 %。 The method for preparing a novel silica powder material according to claim 4, wherein the mass ratio of the hydrolyzable organic substance to the silica sol is from 1% to 25%.
6.根据权利要求 4所述的新型二氧化硅粉体材料的制备方法， 其特征在 于： 通过调节可水解有机物的含量， 可制备出不同粒径的二氧化硅粉体材料。 The method for preparing a novel silica powder material according to claim 4, wherein: the silica powder material having different particle diameters can be prepared by adjusting the content of the hydrolyzable organic substance.
7.根据权利要求 4〜7中任一项所述的新型二氧化硅粉体材料的制备方 法， 其特征在于： 所述可水解有机物为可水解硅垸。
The method for producing a novel silica powder material according to any one of claims 4 to 7, wherein the hydrolyzable organic substance is hydrolyzable silicon germanium.
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| CN86106689A (en) * | 1985-09-25 | 1987-05-27 | 默克专利股份公司 | Preparing spherical SiO 2 particles |
| JPH03258878A (en) * | 1990-03-07 | 1991-11-19 | Nissan Chem Ind Ltd | Coating composition |
| CN1573583A (en) * | 2003-05-13 | 2005-02-02 | 信越化学工业株式会社 | Spherical silica-titania-based fine particles surface-treated with silane, production process and use therefor |
| CN102295292A (en) * | 2010-06-25 | 2011-12-28 | 富士施乐株式会社 | Silica particles and method of producing the same |
-
2012
- 2012-07-03 WO PCT/CN2012/078079 patent/WO2014005272A1/en active Application Filing
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86106689A (en) * | 1985-09-25 | 1987-05-27 | 默克专利股份公司 | Preparing spherical SiO 2 particles |
| JPH03258878A (en) * | 1990-03-07 | 1991-11-19 | Nissan Chem Ind Ltd | Coating composition |
| CN1573583A (en) * | 2003-05-13 | 2005-02-02 | 信越化学工业株式会社 | Spherical silica-titania-based fine particles surface-treated with silane, production process and use therefor |
| CN102295292A (en) * | 2010-06-25 | 2011-12-28 | 富士施乐株式会社 | Silica particles and method of producing the same |
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