CN103360796A - Method for in situ modification of amphoteric nano silica - Google Patents
Method for in situ modification of amphoteric nano silica Download PDFInfo
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- CN103360796A CN103360796A CN2013102580187A CN201310258018A CN103360796A CN 103360796 A CN103360796 A CN 103360796A CN 2013102580187 A CN2013102580187 A CN 2013102580187A CN 201310258018 A CN201310258018 A CN 201310258018A CN 103360796 A CN103360796 A CN 103360796A
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Abstract
The invention relates to a method for in situ modification of amphoteric nano silica and belongs to the technical field of modification of inorganic silicon materials. The method comprises the following steps of: reacting for 1-12 hours at the temperature of 20-180 DEG C to prepare silicone gel in a reactor based on sodium silicate and sulfuric acid as raw materials; adding a coupling agent which serves as a modifying agent; adding one or more of methanol, ethanol, propanol, butanol, ethylene glycol, isobutyl alcohol, tetramethylammonium hydroxide, potassium hydroxide, sodium hydroxide, ammonium hydroxide, hydrochloric acid and acetic acid at the same time, and further reacting for 1-8 hours; washing off sulfate particles, chlorine particles and other particles by using a particle removing water; drying for 2-8 hours at the temperature of 80-1,000 DEG C to obtain modified hydrophobic nano silica powder. The nano silica powder obtained by adopting the novel method for in situ modification and grafting of the amphoteric nano silica can disperse better in aqueous and oily systems, has better dispersibility and can be used more widely.
Description
Technical field:
The present invention relates to inorganic silicon material modification technical field, relate in particular to the in-situ modified mass production production method of new both sexes 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 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 the in-situ modified method of a kind of both sexes nano silicon.Nano silicon is better disperseed in water-based, oiliness system and use, a kind of in-situ modified grafting method of new nano silicon is provided, thus the dispersed better nano silica powder of preparation.
For achieving the above object, the technical solution used in the present invention is:
The in-situ modified method of a kind of both sexes nano silicon is characterized in that the preparation method:
A. take water glass and sulfuric acid as raw material, preparation silicon gel in reactor, temperature of reaction is 20-180 ℃, the reaction times is 1-12 hour;
B. add again coupling agent as properties-correcting agent;
C. add simultaneously one or more in methyl alcohol, ethanol, propyl alcohol, butanols, ethylene glycol, isopropylcarbinol, Tetramethylammonium hydroxide, potassium hydroxide, sodium hydroxide, ammonium hydroxide, hydrochloric acid, the acetic acid, continue reaction 1-8 hour;
D. spend particle washing desulfuration acid group particle, chlorine particle and other particle;
E. 80-1000 ℃ of lower oven dry 2-8 hour, obtain the dewatering nano silicon-dioxide powdery of modification.
Described coupling agent is Silane coupling agent KH550/KH560/KH792/KH151/KH590, and in the macromolecular coupling agent one or more.
Described macromolecular coupling agent is phthalate ester coupling agent or stearic acid.
The invention has the beneficial effects as follows:
The in-situ modified method of a kind of both sexes nano silicon provided by the invention, nano silicon is better disperseed in water-based, oiliness system, Application Areas is more extensive, a kind of in-situ modified grafting method of new nano silicon is provided, thus the dispersed better nano silica powder of preparation.
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
The in-situ modified mass production production method of a kind of both sexes nano silicon,
(1) water glass solution of preparation 10% heats 20 ℃ in reactor, and segmentation adds the vitriol oil or dilute sulphuric acid, 2 hours reaction times, when the pH value is 2, stop to add sulfuric acid, and stirred 1 hour, temperature is 60 ℃;
(2) add Silane coupling agent KH550;
(3) add simultaneously methyl alcohol, continue reaction 2 hours;
(4) spend particle washing desulfuration acid group particle, chlorine particle and other particle, 200 ℃ of lower oven dry 5 hours, obtain the dewatering nano silicon-dioxide powdery of modification.
Embodiment 2
The in-situ modified mass production production method of a kind of both sexes nano silicon,
(1) water glass solution of preparation 15% heats 80 ℃ in reactor, and segmentation adds the vitriol oil or dilute sulphuric acid, 5 hours reaction times, when the pH value is 1-6, stop to add sulfuric acid, and stirred 2.5 hours, temperature is 100 ℃;
(2) add silane coupling agent KH560 and phthalate ester coupling agent;
(3) add simultaneously industrial spirit, continue reaction 1-8 hour;
(4) spend particle washing desulfuration acid group particle, chlorine particle and other particle, 500 ℃ of lower oven dry 5 hours, obtain the dewatering nano silicon-dioxide powdery of modification.
Embodiment 3
The in-situ modified mass production production method of a kind of both sexes nano silicon,
(1) water glass solution of preparation 20% heats 100 ℃ in reactor, and segmentation adds the vitriol oil or dilute sulphuric acid, 8 hours reaction times, when the pH value is 5, stop to add sulfuric acid, and stirred 3 hours, temperature is 110 ℃;
(2) add silane coupling agent KH590;
(3) add simultaneously methyl alcohol and ethanol, continue reaction 8 hours;
(4) spend particle washing desulfuration acid group particle, chlorine particle and other particle, 900 ℃ of lower oven dry 5 hours, obtain the dewatering nano silicon-dioxide powdery of modification.
Above demonstration 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 (3)
1. in-situ modified method of both sexes nano silicon is characterized in that the preparation method:
A. take water glass and sulfuric acid as raw material, preparation silicon gel in reactor, temperature of reaction is 20-180 ℃, the reaction times is 1-12 hour;
B. add again coupling agent as properties-correcting agent;
C. add simultaneously one or more in methyl alcohol, ethanol, propyl alcohol, butanols, ethylene glycol, isopropylcarbinol, Tetramethylammonium hydroxide, potassium hydroxide, sodium hydroxide, ammonium hydroxide, hydrochloric acid, the acetic acid, continue reaction 1-8 hour;
D. spend particle washing desulfuration acid group particle, chlorine particle and other particle;
E. 80-1000 ℃ of lower oven dry 2-8 hour, obtain the dewatering nano silicon-dioxide powdery of modification.
2. the in-situ modified method of both sexes nano silicon according to claim 1, it is characterized in that: described coupling agent is Silane coupling agent KH550/KH560/KH792/KH151/KH590, and in the macromolecular coupling agent one or more.
3. the in-situ modified method of both sexes nano silicon according to claim 2, it is characterized in that: described macromolecular coupling agent is phthalate ester coupling agent or stearic acid.
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| CN2013102580187A CN103360796A (en) | 2013-06-25 | 2013-06-25 | Method for in situ modification of amphoteric nano silica |
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| CN2013102580187A CN103360796A (en) | 2013-06-25 | 2013-06-25 | Method for in situ modification of amphoteric nano silica |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103911022A (en) * | 2014-04-10 | 2014-07-09 | 福建省顺昌县新和纳米硅业有限公司 | Particle size controllable nano silica and preparation method thereof |
| CN104893363A (en) * | 2015-06-05 | 2015-09-09 | 确成硅化学股份有限公司 | Modification method of precipitation-process silica white |
| CN106749948A (en) * | 2016-12-03 | 2017-05-31 | 安徽富丽华化工有限公司 | A kind of heat resist modification unsaturated polyester resin and preparation method thereof |
| CN107140650A (en) * | 2017-04-07 | 2017-09-08 | 河南大学 | A kind of silica nanometer surfactant and preparation method thereof |
| CN114311861A (en) * | 2021-12-28 | 2022-04-12 | 浙江东进新材料有限公司 | Waterproof and antibacterial composite functional fabric |
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| CN102532950A (en) * | 2010-12-17 | 2012-07-04 | 北京航天赛德科技发展有限公司 | Preparation method for microparticle type silica gel thin film opening agent |
| CN102666383A (en) * | 2009-11-16 | 2012-09-12 | 日挥触媒化成株式会社 | Process for production of silica-alumina sol, silica-alumina sol, coating agent for formation of transparent coating film which comprises the sol, and substrate having transparent coating film attached thereto |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103911022A (en) * | 2014-04-10 | 2014-07-09 | 福建省顺昌县新和纳米硅业有限公司 | Particle size controllable nano silica and preparation method thereof |
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| CN104893363A (en) * | 2015-06-05 | 2015-09-09 | 确成硅化学股份有限公司 | Modification method of precipitation-process silica white |
| CN106749948A (en) * | 2016-12-03 | 2017-05-31 | 安徽富丽华化工有限公司 | A kind of heat resist modification unsaturated polyester resin and preparation method thereof |
| CN107140650A (en) * | 2017-04-07 | 2017-09-08 | 河南大学 | A kind of silica nanometer surfactant and preparation method thereof |
| CN114311861A (en) * | 2021-12-28 | 2022-04-12 | 浙江东进新材料有限公司 | Waterproof and antibacterial composite functional fabric |
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Application publication date: 20131023 |