CN103359739A - Method for producing special modified nano silicon dioxide for plastics in large scale - Google Patents
Method for producing special modified nano silicon dioxide for plastics in large scale Download PDFInfo
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- CN103359739A CN103359739A CN201310256181XA CN201310256181A CN103359739A CN 103359739 A CN103359739 A CN 103359739A CN 201310256181X A CN201310256181X A CN 201310256181XA CN 201310256181 A CN201310256181 A CN 201310256181A CN 103359739 A CN103359739 A CN 103359739A
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Abstract
The invention relates to a method for producing special modified nano silicon dioxide for plastics in a large scale, relating to the field of inorganic silicon material modification technologies. The method comprises the following steps of taking sodium silicate and sulfuric acid as the raw material; 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 diluted coupling reagent which is taken as a modifier, wherein the diluent is an alcohol substance; simultaneously adding alkaline matter and acidic material and reacting for 1-8 hours continuously; washing sulfate radical particles, chlorine particles and other particles with deionized water; drying for 7 hours at 80-900 DEG C; and 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 plastic, 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 a kind of modification mass production production method of plastics special-purpose nanometer silicon-dioxide.
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 modification mass production production method of plastics special-purpose nanometer silicon-dioxide.Silicon-dioxide can better better be disperseed to use in conjunction with reaching by the key base in plastics, 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 modification mass production production method of plastics special-purpose nanometer silicon-dioxide is characterized in that step is:
A. take water glass and sulfuric acid as raw material, preparation silicon gel in reactor, temperature is at 20-180 ℃, and the reaction times is 1-12 hour;
B. the coupling agent after the adding dilution is as properties-correcting agent, and thinner is alcohols material;
C. add simultaneously alkaline matter and acidic substance, continue reaction 1-8 hour;
D. spend particle washing desulfuration acid group particle, chlorine particle and other particle;
E. 80-900 ℃ of lower oven dry 7 hours, obtain the dewatering nano silicon-dioxide powdery of modification.
Among the above-mentioned steps a, water glass is mixed with the sodium silicate solution of 6%-30% in reactor, and segmentation adds the vitriol oil or dilute sulphuric acid, to pH be 7-10.
Described coupling agent is Silane coupling agent KH550, KH560, KH151, KH792, and in the macromolecular coupling agent one or more.
Described alcohols material is one or more in propyl alcohol, butanols, the ethylene glycol.
Described alkaline matter is one or more in Tetramethylammonium hydroxide, potassium hydroxide, the sodium hydroxide.
Described acidic substance are one or more in erucicamide, erucic acid, hydrochloric acid, the acetic acid.
The invention has the beneficial effects as follows:
The modification mass production production method of a kind of plastics special-purpose nanometer silicon-dioxide provided by the invention, silicon-dioxide can better better be disperseed to use in conjunction with reaching by the key base in plastics, 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 modification mass production production method of plastics special-purpose nanometer silicon-dioxide,
(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 7, stops to add sulfuric acid, stirs 1 hour, temperature is 30 to spend.
(2) the coupling agent KH550 after adding is diluted with propyl alcohol adds Tetramethylammonium hydroxide and erucicamide simultaneously as properties-correcting agent, continues 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 modification mass production production method of plastics special-purpose nanometer silicon-dioxide,
(1) compound concentration be 20% sodium silicate solution in reactor, segmentation adds the vitriol oil or dilute sulphuric acid, heat 50 ℃, reacts 5 hours, when the pH value is 8, stops to add sulfuric acid, stirs 2 hours, temperature is 60 to spend.
(2) add with the coupling agent KH560 after the butanols dilution as properties-correcting agent, add simultaneously sodium hydroxide etc. and erucic acid, continue reaction 5 hours.
(3) spend particle washing desulfuration acid group particle chlorine particle and other particle, 500 ℃ of lower oven dry 7 hours, obtain the dewatering nano silicon-dioxide powdery of modification.
Embodiment 3
A kind of modification mass production production method of plastics special-purpose nanometer silicon-dioxide,
(1) compound concentration be 30% sodium silicate solution in reactor, segmentation adds the vitriol oil or dilute sulphuric acid, heat 180 ℃, reacts 9 hours, when the pH value is 10, stops to add sulfuric acid, stirs 3 hours, temperature is 130 to spend.
(2) the coupling agent KH151 after adding is diluted with pure ethylene glycol adds potassium hydroxide and acid goods and materials hydrochloric acid simultaneously as properties-correcting agent, continues reaction 8 hours.
(3) spend particle washing desulfuration acid group particle chlorine particle and other particle, 900 ℃ 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 (6)
1. the modification mass production production method of a plastics special-purpose nanometer silicon-dioxide is characterized in that step is:
A. take water glass and sulfuric acid as raw material, preparation silicon gel in reactor, temperature is at 20-180 ℃, and the reaction times is 1-12 hour;
B. the coupling agent after the adding dilution is as properties-correcting agent, and thinner is alcohols material;
C. add simultaneously alkaline matter and acidic substance, continue reaction 1-8 hour;
D. spend particle washing desulfuration acid group particle, chlorine particle and other particle;
E. 80-900 ℃ of lower oven dry 7 hours, obtain the dewatering nano silicon-dioxide powdery of modification.
2. the modification mass production production method of plastics special-purpose nanometer silicon-dioxide according to claim 1, it is characterized in that: among the above-mentioned steps a, water glass is mixed with the sodium silicate solution of 6%-30% in reactor, and segmentation adds the vitriol oil or dilute sulphuric acid, to pH be 7-10.
3. the modification mass production production method of plastics special-purpose nanometer silicon-dioxide according to claim 1 and 2, it is characterized in that: described coupling agent is Silane coupling agent KH550, KH560, KH151, KH792, and in the macromolecular coupling agent one or more.
4. the modification mass production production method of plastics special-purpose nanometer silicon-dioxide according to claim 1 and 2, it is characterized in that: described alcohols material is one or more in propyl alcohol, butanols, the ethylene glycol.
5. the modification mass production production method of plastics special-purpose nanometer silicon-dioxide according to claim 1 and 2, it is characterized in that: described alkaline matter is one or more in Tetramethylammonium hydroxide, potassium hydroxide, the sodium hydroxide.
6. the modification mass production production method of plastics special-purpose nanometer silicon-dioxide according to claim 1 and 2, it is characterized in that: described acidic substance are one or more in erucicamide, erucic acid, hydrochloric acid, the acetic acid.
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| CN201310256181XA CN103359739A (en) | 2013-06-25 | 2013-06-25 | Method for producing special modified nano silicon dioxide for plastics in large scale |
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| CN201310256181XA CN103359739A (en) | 2013-06-25 | 2013-06-25 | Method for producing special modified nano silicon dioxide for plastics in large scale |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN108584966A (en) * | 2018-06-22 | 2018-09-28 | 确成硅化学股份有限公司 | A kind of preparation method of the high reinforcing white carbon of high dispersive |
| CN113372742A (en) * | 2021-05-10 | 2021-09-10 | 广东力达新材料科技有限公司 | Silicate coating and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101659415A (en) * | 2008-08-29 | 2010-03-03 | 山东海纳高科材料有限公司 | Method for producing high-dispersing multi-group amphiphilic nano silicon oxide powder or dispersion |
-
2013
- 2013-06-25 CN CN201310256181XA patent/CN103359739A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101659415A (en) * | 2008-08-29 | 2010-03-03 | 山东海纳高科材料有限公司 | Method for producing high-dispersing multi-group amphiphilic nano silicon oxide powder or dispersion |
Non-Patent Citations (1)
| 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》, vol. 24, 31 December 2007 (2007-12-31), pages 22 - 24 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN108584966A (en) * | 2018-06-22 | 2018-09-28 | 确成硅化学股份有限公司 | A kind of preparation method of the high reinforcing white carbon of high dispersive |
| CN113372742A (en) * | 2021-05-10 | 2021-09-10 | 广东力达新材料科技有限公司 | Silicate coating and preparation method thereof |
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Application publication date: 20131023 |