CN103360795A - Modified production method for nano silicon dioxide for special rubber - Google Patents
Modified production method for nano silicon dioxide for special rubber Download PDFInfo
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- CN103360795A CN103360795A CN2013102561716A CN201310256171A CN103360795A CN 103360795 A CN103360795 A CN 103360795A CN 2013102561716 A CN2013102561716 A CN 2013102561716A CN 201310256171 A CN201310256171 A CN 201310256171A CN 103360795 A CN103360795 A CN 103360795A
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Abstract
The invention relates to a modified production method for nano silicon dioxide for special rubber, relating to the technical field of inorganic silicon material modification. The method is characterized by comprising the following steps of taking sodium silicate and sulfuric acid as the raw material; firstly preparing silica gel in a reaction kettle, wherein the temperature is 20-180 DEG C, and the reaction time is 1-12 hours; adding a coupling reagent KH590 or SI69 which are taken as a modifier; simultaneously adding isobutanol and reacting for 1-8 hours continuously; washing sulfate radical particles, chlorine particles and other particles with deionized water; drying for 8 hours at 80-900 DEG C, thus obtaining the modified hydrophobic nano silicon dioxide powder body. According to the method, the silicon dioxide can be well combined with bond bases and dispersed for application in the rubber, so that the nano silicon dioxide has wider application fields; an in situ modification method for nano silicon dioxide, which has better applicability, is provided, so that nano silicon dioxide powder body with better dispersibility is prepared.
Description
Technical field:
The present invention relates to inorganic silicon material modification technical field, relate in particular to the modified producing method that a kind of specialty elastomer is used nano silicon.
Background technology:
Nano silicon is one of ultra tiny New Inorganic Materials of extremely important high-tech, because of its particle diameter very little, specific surface area is large, surface adsorption power is strong, surface energy is large, and the aspects such as chemical purity is high, dispersing property is good, thermal resistance, resistance have special performance, with its superior stability, reinforcement, thickening property and thixotropy, in numerous subjects and field, show unique characteristics, the effect of not replacing is arranged.Nano silicon is commonly called as " ultra-fine white carbon black ", be widely used in every profession and trade as additive, support of the catalyst, petrochemical complex, discoloring agent, matting agent, rubber reinforcing filler, the plastics filling agent, printing ink thickening material, the soft polishing agent of metal, the insulation and thermal insulation weighting agent, the various fields such as high-grade daily-use makeup filler and spray material, medicine, environmental protection.
The preparation method of nano silicon is divided into two kinds of Physical and chemical methods.Physical technique simply but easily bring impurity into, powdery row material characteristic is difficult to control, preparation efficiency is low and size distribution is wider.Chemical method can make pure and the uniform ultra-fine SiO of size distribution
2Particle, chemical method comprises chemical vapour deposition (CVD) method, liquid phase method, ion exchange method, the precipitator method and collosol and gel (Sol-Gel) method etc. but main production method or the vapor phase process take silicon tetrachloride as raw material, and Ti acid sodium and mineral acid are the precipitator method and the sol-gel method take silicic acid vinegar etc. as raw material of raw material.
The novel silicon material is still in continuous development and application at present, and to prepare the nano silicon product of excellent property, the at present production of China's nano silicon is still relatively backward, and the research work in this field is still waiting to break through.
Summary of the invention:
The object of the present invention is to provide a kind of specialty elastomer modified producing method of nano silicon.Silicon-dioxide can better better be disperseed to use in conjunction with reaching by the key base in rubber, the in-situ modified method of the more intense nano silicon of a kind of suitability is provided.
For achieving the above object, the technical solution used in the present invention is:
A kind of specialty elastomer modified producing method of nano silicon, it is characterized in that step is: take water glass and sulfuric acid as raw material, at first in reactor, prepare the silicon gel, temperature is at the 20-180 degree, reaction times is 1-12 hour, add coupling agent KH590 or SI69 as properties-correcting agent, add simultaneously isopropylcarbinol, continue reaction 1-8 hour; Spend particle washing desulfuration acid group particle, chlorine particle and other particle, 80-900 ℃ of lower oven dry 8 hours, obtain the dewatering nano silicon-dioxide powdery of modification.
The invention has the beneficial effects as follows:
A kind of specialty elastomer provided by the invention modified producing method of nano silicon, silicon-dioxide can better better be disperseed to use in conjunction with reaching by the key base in rubber, Application Areas is more extensive, the in-situ modified method of the more intense nano silicon of a kind of suitability is provided, thereby makes dispersed better nano silica powder.
Embodiment:
For technique means, creation characteristic that the present invention is realized, reach purpose and effect is easy to understand, below in conjunction with concrete specific embodiment, further set forth the present invention, but be not to limit protection scope of the present invention.
Embodiment 1
A kind of specialty elastomer modified producing method of nano silicon,
(1) compound concentration be 6% sodium silicate solution in reactor, segmentation adds the vitriol oil or dilute sulphuric acid, heat 30 ℃, reacts 2 hours, when the pH value is 8, stops to add sulfuric acid, stirs 1 hour, temperature is 30 to spend.
(2) add coupling agent KH590 as properties-correcting agent, add simultaneously isopropylcarbinol, continue reaction 2 hours.
(3) spend particle washing desulfuration acid group particle chlorine particle and other particle, 100 ℃ of lower oven dry 7 hours, obtain the dewatering nano silicon-dioxide powdery of modification.
Embodiment 2
A kind of specialty elastomer modified producing method of nano silicon,
(1) compound concentration be 6% sodium silicate solution in reactor, segmentation adds the vitriol oil or dilute sulphuric acid, heat 30 ℃, reacts 2 hours, when the pH value is 8, stops to add sulfuric acid, stirs 1 hour, temperature is 30 to spend.
(2) add coupling agent SI69 as properties-correcting agent, add simultaneously isopropylcarbinol, continue reaction 2 hours.
(3) spend particle washing desulfuration acid group particle chlorine particle and other particle, 100 ℃ of lower oven dry 7 hours, obtain the dewatering nano silicon-dioxide powdery of modification.
More than show and described ultimate principle of the present invention, principal character and advantage of the present invention.It only is the specific embodiment of the present invention; but protection scope of the present invention is not limited to this; any those of ordinary skill in the art are in the disclosed technical scope of the present invention, and the variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (1)
1. a specialty elastomer is with the modified producing method of nano silicon, it is characterized in that step is: take water glass and sulfuric acid as raw material, at first in reactor, prepare the silicon gel, temperature is at the 20-180 degree, reaction times is 1-12 hour, add coupling agent KH590 or SI69 as properties-correcting agent, add simultaneously isopropylcarbinol, continue reaction 1-8 hour; Spend particle washing desulfuration acid group particle, chlorine particle and other particle, 80-900 ℃ of lower oven dry 8 hours, obtain the dewatering nano silicon-dioxide powdery of modification.
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| CN2013102561716A CN103360795A (en) | 2013-06-25 | 2013-06-25 | Modified production method for nano silicon dioxide for special rubber |
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| CN2013102561716A CN103360795A (en) | 2013-06-25 | 2013-06-25 | Modified production method for nano silicon dioxide for special rubber |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104031426A (en) * | 2014-05-12 | 2014-09-10 | 谷屿 | Surface-modified nanometer titanium dioxide and preparation method thereof |
| CN109306129A (en) * | 2018-09-11 | 2019-02-05 | 武汉大学 | A kind of cable insulating layer material of modified sulfur-bearing nano silica enhancing and its application |
| CN109439022A (en) * | 2018-11-16 | 2019-03-08 | 江苏师范大学 | A kind of high oil-absorbing white carbon black |
| CN111807379A (en) * | 2020-07-15 | 2020-10-23 | 确成硅化学股份有限公司 | Low-hysteresis high-dispersion white carbon black and preparation method thereof |
| CN112341667A (en) * | 2020-12-01 | 2021-02-09 | 甘肃中科凯越硅材料科技有限公司 | Preparation of modified silicon micropowder and application of modified silicon micropowder in polymer composite material |
| CN112552709A (en) * | 2020-12-29 | 2021-03-26 | 无锡恒诚硅业有限公司 | Preparation method of surface modified silicon dioxide |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5965202A (en) * | 1996-05-02 | 1999-10-12 | Lucent Technologies, Inc. | Hybrid inorganic-organic composite for use as an interlayer dielectric |
| EP1295850A1 (en) * | 2001-09-20 | 2003-03-26 | Degussa AG | Precipitated silica with a high BET/CTAB specific area ratio |
| CN1536032A (en) * | 2003-04-07 | 2004-10-13 | 章浩龙 | Nano silicon dioxide emulsion, its preparation method and application |
| CN101585539A (en) * | 2009-06-25 | 2009-11-25 | 福建省漳平市正盛化工有限公司 | Prepartion method of highly anti-yellow resistance white carbon black for silastic |
| CN101633797A (en) * | 2008-07-24 | 2010-01-27 | 中国石油天然气股份有限公司 | Surface modified nano silicon oxide |
| CN101979443A (en) * | 2010-10-12 | 2011-02-23 | 四川久大制盐有限责任公司 | Method for producing modified white carbon black |
| CN102229758A (en) * | 2011-04-06 | 2011-11-02 | 福建正盛无机材料股份有限公司 | Preparation method of high dispersed white carbon black |
| CN102863823A (en) * | 2012-09-19 | 2013-01-09 | 常州大学 | Preparation method of modified nano silicon dioxide |
| CN102911530A (en) * | 2012-11-07 | 2013-02-06 | 北京化工大学 | Preparation method capable of realizing chemical blending of modified nano silicon dioxide particles in acrylate monomer |
| CN102964881A (en) * | 2012-12-07 | 2013-03-13 | 北京彤程创展科技有限公司 | Amino/mercapto silane modified silica and preparation method thereof |
-
2013
- 2013-06-25 CN CN2013102561716A patent/CN103360795A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5965202A (en) * | 1996-05-02 | 1999-10-12 | Lucent Technologies, Inc. | Hybrid inorganic-organic composite for use as an interlayer dielectric |
| EP1295850A1 (en) * | 2001-09-20 | 2003-03-26 | Degussa AG | Precipitated silica with a high BET/CTAB specific area ratio |
| CN1536032A (en) * | 2003-04-07 | 2004-10-13 | 章浩龙 | Nano silicon dioxide emulsion, its preparation method and application |
| CN101633797A (en) * | 2008-07-24 | 2010-01-27 | 中国石油天然气股份有限公司 | Surface modified nano silicon oxide |
| CN101585539A (en) * | 2009-06-25 | 2009-11-25 | 福建省漳平市正盛化工有限公司 | Prepartion method of highly anti-yellow resistance white carbon black for silastic |
| CN101979443A (en) * | 2010-10-12 | 2011-02-23 | 四川久大制盐有限责任公司 | Method for producing modified white carbon black |
| CN102229758A (en) * | 2011-04-06 | 2011-11-02 | 福建正盛无机材料股份有限公司 | Preparation method of high dispersed white carbon black |
| CN102863823A (en) * | 2012-09-19 | 2013-01-09 | 常州大学 | Preparation method of modified nano silicon dioxide |
| CN102911530A (en) * | 2012-11-07 | 2013-02-06 | 北京化工大学 | Preparation method capable of realizing chemical blending of modified nano silicon dioxide particles in acrylate monomer |
| CN102964881A (en) * | 2012-12-07 | 2013-03-13 | 北京彤程创展科技有限公司 | Amino/mercapto silane modified silica and preparation method thereof |
Non-Patent Citations (6)
| Title |
|---|
| 倪文等: "以工业水玻璃为原料制备纳米孔SiO2气凝胶块体材料", 《河南化工》 * |
| 崔益顺: "沉淀二氧化硅表面改性工艺条件优化", 《无机盐工业》 * |
| 滕进丽等: "表面改性SiO_2纳米微粒的表征及摩擦学性能", 《材料科学与工程学报》 * |
| 王艳玲等: "巯基硅烷偶联剂对白炭黑物化性质的影响研究", 《无机盐工业》 * |
| 肖喜庆等: "活性水中改性纳米SiO_2的制备及分散性研究", 《特种油气藏》 * |
| 范淑红等: "制备纳米SiO2的配方优化", 《湖南工业大学学报》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104031426A (en) * | 2014-05-12 | 2014-09-10 | 谷屿 | Surface-modified nanometer titanium dioxide and preparation method thereof |
| CN104031426B (en) * | 2014-05-12 | 2015-05-13 | 谷屿 | Surface-modified nanometer titanium dioxide and preparation method thereof |
| CN109306129A (en) * | 2018-09-11 | 2019-02-05 | 武汉大学 | A kind of cable insulating layer material of modified sulfur-bearing nano silica enhancing and its application |
| CN109439022A (en) * | 2018-11-16 | 2019-03-08 | 江苏师范大学 | A kind of high oil-absorbing white carbon black |
| CN111807379A (en) * | 2020-07-15 | 2020-10-23 | 确成硅化学股份有限公司 | Low-hysteresis high-dispersion white carbon black and preparation method thereof |
| CN111807379B (en) * | 2020-07-15 | 2023-10-27 | 确成硅化学股份有限公司 | Low-hysteresis high-dispersion white carbon black and preparation method thereof |
| CN112341667A (en) * | 2020-12-01 | 2021-02-09 | 甘肃中科凯越硅材料科技有限公司 | Preparation of modified silicon micropowder and application of modified silicon micropowder in polymer composite material |
| CN112552709A (en) * | 2020-12-29 | 2021-03-26 | 无锡恒诚硅业有限公司 | Preparation method of surface modified silicon dioxide |
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Application publication date: 20131023 |