CN1865137A - Nano silicon dioxide preparation method - Google Patents
Nano silicon dioxide preparation method Download PDFInfo
- Publication number
- CN1865137A CN1865137A CN 200510046482 CN200510046482A CN1865137A CN 1865137 A CN1865137 A CN 1865137A CN 200510046482 CN200510046482 CN 200510046482 CN 200510046482 A CN200510046482 A CN 200510046482A CN 1865137 A CN1865137 A CN 1865137A
- Authority
- CN
- China
- Prior art keywords
- preparation
- oil
- water
- alkali metal
- consumption
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Abstract
This invention discloses a method for producing nanometer silica dioxide particle. The procedures comprise: add the alkali metal metasilicate into the mixture of hydrocarbons component, surfactant and cosurfactant to form the nanometer super solubilizing colloidal group system of oil-coated high concentration alkali metal metasilicate, which limits the produced nanometer silica dioxide in the nanometer colloidal group for precipitation reaction, and then the invented nanometer silica dioxide can be obtained by washing and drying. By using the characteristic of the highly internal phase dispersed system of oil-coated high concentration alkali metal metasilicate which can in-situ synthesize nanometer particles, the particle diameter of the produced silica dioxide can be 1-100nm, with a narrow range and single distribution state. This invention is characterized of low consumption of surfactant and hydrocarbon component, and low cost.
Description
Technical field
The present invention relates to a kind of preparation method of superfine silicon dioxide, particularly relate to a kind of preparation method of nanometer silicon dioxide particle.
Background technology
Superfine silicon dioxide is the quality matetrial of electronic ceramics, transparent toothpaste filler, support of the catalyst and loading material of rubber, particularly nano level silicon-dioxide.The preparation method of superfine silicon dioxide has sol-gel method, the precipitator method etc.CN1032641C discloses a kind of method that adopts direct precipitation method to prepare silicon-dioxide, is the silicon source with water glass wherein, and mineral acid is a precipitation agent.CN 1040200C has proposed a kind of segmentation and has added the sedimentary method of mineral acid and prepare silicon-dioxide.CN1036990C discloses a kind of preparation method who is used for the precipitated silica of rubber accelerator, this method is as follows: react under 60-95 ℃ of temperature with alkalimetal silicate and mineral acid, during reaction keeping the pH value is that 7.5-10.5 and continuously stirring reaction last till that solids concn reaches 90-120g/l adjustment pH value to being less than or equal to 5 in sedimentary suspension is arranged, and leaches precipitation, washing, drying and grinds this precipitated silica in case of necessity.The granularity of prepared silicon dioxide granule is all bigger in the above-mentioned patent.
CN 1051054C (97125800.7) litre a kind of method for preparing nanometer silicon dioxide particle from alkali-metal silicate, this method is as follows: prepare alkali metal silicate aqueous solution earlier, the non-polar organic solvent solution and the acidated polar organic solvent that contain tensio-active agent, under the alkali metal silicate aqueous solution agitation condition, add the non-polar organic solvent solution that contains tensio-active agent then, make the inverse micellar solution of alkalimetal silicate, this inverse micellar solution joins in the acidated polar organic solvent again, ageing, centrifugation, make silica dioxide granule, particle diameter is 5～100nm.This method has been to use a large amount of tensio-active agents and non-polar organic solvent, and alkali metal silicate aqueous solution contains a large amount of water simultaneously, and this method is used the exhibiting high surface promoting agent, and cost is higher.
Summary of the invention
For overcoming deficiency of the prior art, the purpose of this invention is to provide the preparation method of nano silicon dioxide that a kind of cost is low, product purity is high and productive rate is high.
The contriver finds through a large amount of experiments, the alkalimetal silicate of high density can be solubilized in hydrocarbon component and the surfactant mixtures, form the super solubilising nanometer micelle of oil bag alkalimetal silicate, control reaction with the nanometer micelle, reaction, the weathering process of alkalimetal silicate and precipitation agent are all carried out in the nanometer micelle, thereby produce nanometer silicon dioxide particle.
The present invention prepares nanometer silicon dioxide particle and comprises the steps:
(1) alkali metal silicate aqueous solution is slowly joined in the mixture of the hydrocarbon component, tensio-active agent and the cosurfactant that are heated to 60～95 ℃, and stir;
(2) in the mixture of step (1) gained, add precipitation agent, continuously stirring is fully reacted it, and the pH value is 7.5～10.5 between the maintenance reaction period, no longer increases up to precipitation, adjust the pH value with precipitation agent then and be less than or equal to 5, obtain the nano silicon precipitation;
(3) nano silicon of gained precipitation obtains nano silicon through washing, drying.
Weight with the mixture of step (1) gained is benchmark, the content of alkalimetal silicate (butt) and water is 70wt%～95wt%, be preferably 80wt%～95wt%, the water yield is 30wt%～55wt%, the hydrocarbon component consumption is 3wt%～22wt%, better be 3.5wt%～8wt%, preferably 4wt%～6wt%.The consumption of tensio-active agent is 0.1wt%～8wt%, better is 0.5wt%～4wt%, preferably 0.8wt%～2wt%.The consumption of cosurfactant is 0～2.0wt%, better is 0～1.0wt%, preferably 0～0.5wt%.
Alkali metal silicate aqueous solution described in the step (1) can adopt commercially available water glass, and the content of silicon oxide is 25～45wt% in the preferably water glass, and modulus is 1.8～3.7.
When if institute's water content exceeds above-mentioned requirements in the described alkali metal silicate aqueous solution, can adopt following at least a method to remove water: a, portion water to be sloughed in alkali metal silicate aqueous solution heating earlier, b, remove portion water with the mixture mixing post-heating of hydrocarbon component, tensio-active agent and cosurfactant at alkali metal silicate aqueous solution.
Tensio-active agent of the present invention be the VB value less than 1 water-in-oil-type tensio-active agent, be selected from SP-40, SP-60, SP-65, SP-80, SP-85, M-201, fatty acid monoglyceride and two sweet esters, ethylene glycol monostearate, glycol ether monostearate, propyleneglycoles list dodecyl ester, polyisobutenyl maleic anhydride polyol ester, hydramine ester emulsifying agent and the succimide class emulsifying agent one or more.Relevant VB value notion please refer to " A Study of Identifying Emulsion Type ofSurfactant--Volume Balance Value " that this patent people is published in the Journal of colloid andinterface science fourth phase in 2002.
Hydrocarbon component used in the present invention is selected from one or more in atmosphere 3rd side cut distillate, vacuum distillate, decompression slack wax, residual oil slack wax, deasphalted oil, vegetables oil and the animal oil.Wherein vacuum distillate is vacuum 1st side cut distillate, second line of distillation distillate, subtracts three-way distillate, subtracts the dewaxing of four line distillates or in the wax-containing distillate one or more, can come from paraffinic base, intermediate base or naphthenic base crude; The decompression slack wax is vacuum 1st side cut distillate, second line of distillation distillate, subtracts three-way distillate, subtracts one or more slack waxs that obtain in the four line distillates, as being the second line of distillation slack wax, subtracting three-way slack wax, subtracting four line slack waxs or its mixture; The residual oil slack wax is the slack wax of frivolous asphalt oil or heavy deasphalted oil.Vegetables oil is selected from one or more in soya-bean oil, peanut oil, rape seed oil, Viscotrol C, Oleum Helianthi, Oleum Cocois and the plam oil; Animal oil is selected from one or more in butter, sheep oil and the lard.
The present invention prepares the used cosurfactant of silicon-dioxide and is selected from petroleum sodium sulfonate, calcium mahogany sulfonate, barium mahogany sulfonate, sodium stearate, sodium oleate, potassium stearate, potassium oleate, Yelkin TTS, phosphoric acid fat, fatty alcohol-polyoxyethylene ether (10), aliphatic acid polyethenoxy ether (15), alkylphenol polyoxyethylene (7), aliphatic amine polyoxyethylene ether (15), polyoxyethylene glycol (400), Yatall MA acid amides, sodium laurylsulfonate and the dodecyl alcohol acyl phosphoric acid ester one or more.
Used precipitation agent is a mineral acid in the inventive method step (2), is selected from nitric acid, sulfuric acid, hydrochloric acid, phosphoric acid and the perchloric acid one or more, preferably adopts the inorganic acid aqueous solution of high density, preferably the vitriol oil.
The median size of the nano silicon of gained of the present invention is 1-100nm, is preferably 7-40nm.Median size wherein is the mean diameter that obtains with the analysis of X-ray grating spectrum.
The inventive method has the following advantages:
1, the inventive method is to utilize the character of super mutually solubilising micelle dispersion system in the height that oil bag high concentration alkali metal silicate can form, and this system is a kind of nanometer original position synthetic technology.
2, the silicon-dioxide particle size distribution range of the inventive method preparation is narrow, is monodisperse status.
3, adopt the high concentration alkali metal silicate in the inventive method, the productive rate height of silicon-dioxide, and used tensio-active agent and hydrocarbon component consumption are little, cost is low.
4, the inventive method technology is simple, can carry out industrial production in enormous quantities.
Embodiment
It is as follows that the present invention prepares the nano silicon concrete steps:
(1) alkali metal silicate aqueous solution is slowly joined in the mixture of the hydrocarbon component, tensio-active agent and the cosurfactant that are heated to 60～95 ℃, and stir, the time of mixing is 1～60 minute; If in the alkali metal silicate aqueous solution during contained hypervolia, preferably alkali metal silicate aqueous solution is removed the moisture of 5～40wt%, and/or after mixing with hydrocarbon component, tensio-active agent and cosurfactant, reheat is removed the 5wt%～80wt% of surplus water.Described heating removal process can adopt common heating method to dewater, and preferably adopts following method to dewater: 0～-the 0.09MPa vacuum condition under, under 60～95 ℃ of temperature, dewater.
(2) in the mixture of step (1) gained, add precipitation agent, become the glue temperature to be controlled at 60～90 ℃, continuously stirring is fully reacted it, and the pH value is 7.5～10.5 between the maintenance reaction period, no longer increase up to precipitation, adjust the pH value with precipitation agent then and be less than or equal to 5, obtain the nano silicon precipitation;
(3) nano silicon of gained precipitation obtains nano silicon through washing, drying.
Washing described in the step of the present invention (3) is to be washed with water to the negatively charged ion weight concentration earlier less than 0.5%, removes part hydrocarbon component and tensio-active agent, uses organic solvent washing then 1～6 time.Used organic solvent has ethanol or acetone.Described drying conditions is :-0.01～-the 0.09MPa vacuum condition under, under 30～80 ℃ of temperature, dewatered 1～5 hour, be preferably at CO
2Super critical condition is dry down.
Further specify method of the present invention below in conjunction with specific embodiment.
The character of each embodiment gained silica product sees Table 2.
Table 1 embodiment of the invention oil phase feedstock property
| Condensation point, ℃ | Oleaginousness, wt% | Viscosity (100 ℃), mm 2/s | Penetration degree (25 ℃), 1/10mm | |
| Atmosphere 3rd side cut oil | 5 | 90 | 2.01 | / |
| First vacuum side stream | 30 | 80 | 4.98 | / |
| Subtract three-way pressed oil | 37 | 68 | 5.55 | / |
| Subtract four line oil | 42 | 56 | 8.58 | 46 |
| Subtract three-way slack wax | 53 | 8.5 | 5.02 | 19 |
| Subtract four line slack waxs | 56.5 | 22 | 6.08 | 25 |
| Frivolous asphalt oil | 38 | 72 | 8.82 | / |
Embodiment 1
(the silicon oxide weight content is 25% with 900g water glass, modulus is 2.8) ebuillition of heated removes portion water to 750g, the 50g that slowly adds 75 ℃ subtracts in the mixture of three-way pressed oil, 7g polyisobutenyl toxilic acid glyceryl ester and 13g T-154, and under this temperature, mixed 20 minutes, under-0.06MPa vacuum condition, remove 150g water; The hydrochloric acid reaction of adding 36% in said mixture, keeping the pH value of mixture is 8.5, no longer increases up to precipitation to make it keep the solubilising state, mixes; Adding fast 36% hydrochloric acid again, to adjust the pH value be 4, and thorough mixing makes and reacts completely again; Be washed with distilled water to sodium-chlor less than 0.5wt%, centrifugation is used washing with alcohol 3 times then, removes most of hydrocarbon component and tensio-active agent, at last under-0.05MPa vacuum condition, 90 ℃ dry 4 hours down, obtain nano silicon of the present invention.Nano silicon median size 30nm.
Embodiment 2
(the silicon oxide weight content is 27% with 1000g water glass, modulus is 2.2) ebuillition of heated removes portion water to 850g, the 40g that slowly adds 75 ℃ subtracts in the mixture of four line oil, 5g polyisobutenyl toxilic acid triethanolamine ester, and under this temperature, mixed 10 minutes, under-0.02MPa vacuum condition, remove 220g water; The sulfuric acid reaction of adding 95% in said mixture, keeping the pH value of mixture is 9, no longer increases up to precipitation to make it keep the solubilising state, mixes; Adding fast 36% hydrochloric acid again, to adjust the pH value be 5, and thorough mixing makes and reacts completely again; Be washed with distilled water to sulfate ion less than 0.5wt%, centrifugation is used washing with alcohol 2 times then, remove most of hydrocarbon component and tensio-active agent, at last under-0.09MPa vacuum condition, 100 ℃ dry 3 hours down, obtain nano silicon of the present invention.The nano silicon median size is 30nm.
Embodiment 3
(the silicon oxide weight content is 25% with 850g water glass, modulus is 2.8) ebuillition of heated removes portion water to 750g, the 30g atmosphere 3rd side cut pressed oil, the 60g that slowly add 75 ℃ subtract in the mixture of three-way slack wax and 60gT-154, and under this temperature, mixed 20 minutes, under-0.06MPa vacuum condition, remove 150g water; Add 98% sulfuric acid reaction in said mixture, keeping the pH value of mixture is 8.5, no longer increases up to precipitation to make it keep the solubilising state, mixes; Adding fast 36% hydrochloric acid again, to adjust the pH value be 4, and thorough mixing makes and reacts completely again; Be washed with distilled water to sodium-chlor less than 0.5wt%, centrifugation is used washing with alcohol 3 times then, removes most of hydrocarbon component and tensio-active agent, at last under-0.05MPa vacuum condition, 90 ℃ dry 4 hours down, obtain nano silicon of the present invention.Nano silicon median size 28nm.
Embodiment 4
(the silicon oxide weight content is 27% with 919g water glass, modulus is 2.2) ebuillition of heated removes portion water to 850g, the 20g first vacuum side stream, the 10g that slowly add 75 ℃ subtract in the mixture of four line slack waxs, the frivolous asphalt oil of 30g, 1gT-155 and 20g Yatall MA acid amides, and under this temperature, mixed 10 minutes, under-0.02MPa vacuum condition, remove 220g water; The sulfuric acid reaction of adding 98% in said mixture, keeping the pH value of mixture is 9, no longer increases up to precipitation to make it keep the solubilising state, mixes; Adding fast 36% hydrochloric acid again, to adjust the pH value be 5, and thorough mixing makes and reacts completely again; Be washed with distilled water to sulfate ion less than 0.5wt%, centrifugation is used washing with alcohol 2 times then, remove most of hydrocarbon component and tensio-active agent, at last under-0.09MPa vacuum condition, 100 ℃ dry 3 hours down, obtain nano silicon of the present invention.Nano silicon median size 40nm.
Table 2 embodiment 1～4 forms and performance
| The character of silicon-dioxide | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| Median size, nm | 34 | 30 | 28 | 40 |
| The BET specific surface, m 2/g | 220 | 250 | 340 | 180 |
Claims (20)
1, a kind of preparation method of nanometer silicon dioxide particle comprises the steps:
(1) alkali metal silicate aqueous solution is slowly joined in the mixture of the hydrocarbon component, tensio-active agent and the cosurfactant that are heated to 60～95 ℃, and stir;
(2) in the mixture of step (1) gained, add precipitation agent, continuously stirring is fully reacted it, and the pH value is 7.5～10.5 between the maintenance reaction period, no longer increases up to precipitation, adjust the pH value with precipitation agent then and be less than or equal to 5, obtain the nano silicon precipitation;
(3) nano silicon of gained precipitation obtains nano silicon through washing, drying;
Weight with the mixture of step (1) gained is benchmark, the consumption of alkalimetal silicate (butt) and water is 70wt%～95wt%, the water yield is 30wt%～55wt%, the hydrocarbon component consumption is 3wt%～22wt%, the consumption of tensio-active agent is 0.1wt%～8wt%, and the consumption of cosurfactant is 0～2.0wt%.
2, preparation method according to claim 1, it is characterized in that the weight with the mixture of step (1) gained is benchmark, the consumption of alkalimetal silicate (butt) and water is 80wt%～95wt%, the water yield is 35wt%～50wt%, the hydrocarbon component consumption is 3.5wt%～8wt%, the consumption of tensio-active agent is 0.5wt%～4wt%, and the consumption of cosurfactant is 0～1.0wt%.
3, preparation method according to claim 1, it is characterized in that the weight with the mixture of step (1) gained is benchmark, the hydrocarbon component consumption is 4wt%～6wt%, and the consumption of tensio-active agent is 0.8wt%～2wt%, and the consumption of cosurfactant is 0～0.5wt%.
4, preparation method according to claim 1 is characterized in that the alkali metal silicate aqueous solution described in the step (1) is a water glass, and wherein the content of silicon oxide is 25wt%～45wt%, and modulus is 1.8-3.7.
5, according to claim 1 or 4 described preparation methods, it is characterized in that if in the used alkali metal silicate aqueous solution during hypervolia, can adopt following at least a method to remove water: a, portion water to be sloughed in alkali metal silicate aqueous solution heating earlier, b, remove portion water with the mixture mixing post-heating of hydrocarbon component, tensio-active agent and cosurfactant at alkali metal silicate aqueous solution.
6, preparation method according to claim 5 is characterized in that the method that the water yield is met the demands is as follows: the water of alkali metal silicate aqueous solution heating earlier being sloughed 5wt%-40wt%; Alkali metal silicate aqueous solution mixes 5wt%～80wt% that the back reheat is removed remainder water with the mixture of hydrocarbon component, tensio-active agent and cosurfactant.
7, preparation method according to claim 1 is characterized in that described tensio-active agent is selected from one or more in SP-40, SP-60, SP-65, SP-80, SP-85, M-201, fatty acid monoglyceride and two sweet esters, ethylene glycol monostearate, glycol ether monostearate, propyleneglycoles list dodecyl ester, polyisobutenyl maleic anhydride polyol ester, hydramine ester emulsifying agent and the succimide class emulsifying agent.
8, preparation method according to claim 1 is characterized in that employed hydrocarbon component is selected from one or more in atmosphere 3rd side cut distillate, vacuum distillate, decompression slack wax, residual oil slack wax, deasphalted oil, vegetables oil and the animal oil.
9, preparation method according to claim 8 is characterized in that described vacuum distillate is vacuum 1st side cut distillate, second line of distillation distillate, subtracts three-way distillate, subtracts the dewaxing of four line distillates or in the wax-containing distillate one or more; The decompression slack wax is vacuum 1st side cut distillate, second line of distillation distillate, subtracts three-way distillate, subtracts one or more slack waxs that obtain in the four line distillates; The residual oil slack wax is the slack wax of frivolous asphalt oil or heavy deasphalted oil; Vegetables oil is selected from one or more in soya-bean oil, peanut oil, rape seed oil, Viscotrol C, Oleum Helianthi, Oleum Cocois and the plam oil; Animal oil is selected from one or more in butter, sheep oil and the lard.
10, preparation method according to claim 1 is characterized in that described cosurfactant is selected from one or more in petroleum sodium sulfonate, calcium mahogany sulfonate, barium mahogany sulfonate, sodium stearate, sodium oleate, potassium stearate, potassium oleate, Yelkin TTS, phosphoric acid fat, fatty alcohol-polyoxyethylene ether (10), aliphatic acid polyethenoxy ether (15), alkylphenol polyoxyethylene (7), aliphatic amine polyoxyethylene ether (15), polyoxyethylene glycol (400), Yatall MA acid amides, sodium laurylsulfonate and the dodecyl alcohol acyl phosphoric acid ester.
11, preparation method according to claim 1 is characterized in that used precipitation agent in the described step (2) is one or more in nitric acid, sulfuric acid, hydrochloric acid, phosphoric acid and the perchloric acid.
12, preparation method according to claim 1 is characterized in that described precipitation agent is the vitriol oil.
13, preparation method according to claim 1, the median size that it is characterized in that the nano silicon of gained is 1-100nm.
14, preparation method according to claim 1, the median size that it is characterized in that the nano silicon of gained is 7-40nm.
15, preparation method according to claim 1, it is characterized in that in the described step (1), it is as follows to mix the method that post-heating dewaters :-0.01～-the 0.09MPa vacuum condition under, under 60～95 ℃ of temperature, constantly stir the 5wt%～80wt% that removes remainder water.
16, preparation method according to claim 1 is characterized in that control reaction temperature is 60～90 ℃ in the step (2).
17, preparation method according to claim 1 is characterized in that the described washing process of step (3) is as follows: be washed with water to the negatively charged ion weight concentration less than 0.5%.
18, preparation method according to claim 1 is characterized in that the washing process described in the step (3) is as follows: be washed with water to the negatively charged ion weight concentration less than 0.5%, use organic solvent washing again 1～6 time, used organic solvent is ethanol or acetone.
19, preparation method according to claim 1, it is characterized in that the drying described in the step (3) be-0.01～-the 0.09MPa vacuum condition under, under 30～80 ℃ of temperature, dewatered 1～5 hour.
20, preparation method according to claim 19 is characterized in that the drying described in the step (3) is at CO
2Carry out under the super critical condition.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100464825A CN100345755C (en) | 2005-05-18 | 2005-05-18 | Nano silicon dioxide preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100464825A CN100345755C (en) | 2005-05-18 | 2005-05-18 | Nano silicon dioxide preparation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1865137A true CN1865137A (en) | 2006-11-22 |
| CN100345755C CN100345755C (en) | 2007-10-31 |
Family
ID=37424311
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100464825A Active CN100345755C (en) | 2005-05-18 | 2005-05-18 | Nano silicon dioxide preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100345755C (en) |
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102451673A (en) * | 2010-10-15 | 2012-05-16 | 中国石油化工股份有限公司 | Preparation method of nanometer silicon hydroxide-aluminum hydroxide powder |
| CN102451767A (en) * | 2010-10-15 | 2012-05-16 | 中国石油化工股份有限公司 | Method for preparing alumina carrier |
| CN101890371B (en) * | 2009-05-19 | 2012-08-29 | 中国石油化工股份有限公司 | Titanium dioxide-aluminum oxide composite carrier and preparation method thereof |
| CN103449454A (en) * | 2013-09-18 | 2013-12-18 | 武汉科技大学 | Method for preparing nano silicon dioxide by using bamboo leaves as materials and nano silicon dioxide prepared by method |
| CN104030302A (en) * | 2014-06-16 | 2014-09-10 | 深圳迈思瑞尔科技有限公司 | Method for preparing silicon dioxide pellets |
| CN104341568A (en) * | 2013-07-26 | 2015-02-11 | 五邑大学 | Preparation method of nanometer silica polyether (ester) polyol dispersion for modifying polyurethane |
| CN104556076A (en) * | 2015-02-03 | 2015-04-29 | 苏州纳迪微电子有限公司 | Preparation method of ultrahigh-purity amorphous spherical silica powder |
| CN104891506A (en) * | 2015-06-05 | 2015-09-09 | 确成硅化学股份有限公司 | Manufacturing method of low-BET high-dispersivity silica white |
| CN105000567A (en) * | 2015-07-30 | 2015-10-28 | 西南石油大学 | Preparation method for high-dispersity nano-silica |
| CN106147892A (en) * | 2016-07-26 | 2016-11-23 | 深圳市前海龙达新能源有限公司 | A kind of white oil nanometer additive, preparation method and modified white oil thereof |
| CN106378056A (en) * | 2016-08-27 | 2017-02-08 | 安徽龙泉硅材料有限公司 | Pigment dispersing agent prepared by amphiphilic precipitated silica |
| CN106381087A (en) * | 2016-08-27 | 2017-02-08 | 安徽龙泉硅材料有限公司 | Preparation method of precipitated silica for water-based adhesive |
| CN108017061A (en) * | 2017-12-06 | 2018-05-11 | 上海应用技术大学 | One kind prepares large-specific surface area nano SiO using waterglass2Method |
| CN108069430A (en) * | 2017-12-28 | 2018-05-25 | 无锡恒诚硅业有限公司 | A kind of preparation method of high dispersive precipitated silica and precipitated silica therefrom |
| CN109399639A (en) * | 2018-12-10 | 2019-03-01 | 中国医科大学 | A kind of preparation method of regulation ball shaped nano silicon particle and spherical mesoporous silicon nanoparticle |
| CN113789042A (en) * | 2021-11-03 | 2021-12-14 | 广东特普爱高分子材料有限公司 | Flame-retardant environment-friendly PC-ABS composite plastic master batch and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SE501214C2 (en) * | 1992-08-31 | 1994-12-12 | Eka Nobel Ab | Silica sol and process for making paper using the sun |
| CN1051054C (en) * | 1997-12-30 | 2000-04-05 | 中国科学院感光化学研究所 | Process for preparing nm silicon dioxide granule from alkali metal silicate |
-
2005
- 2005-05-18 CN CNB2005100464825A patent/CN100345755C/en active Active
Cited By (24)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101890371B (en) * | 2009-05-19 | 2012-08-29 | 中国石油化工股份有限公司 | Titanium dioxide-aluminum oxide composite carrier and preparation method thereof |
| CN102451767A (en) * | 2010-10-15 | 2012-05-16 | 中国石油化工股份有限公司 | Method for preparing alumina carrier |
| CN102451767B (en) * | 2010-10-15 | 2013-08-28 | 中国石油化工股份有限公司 | Method for preparing alumina carrier |
| CN102451673B (en) * | 2010-10-15 | 2014-07-23 | 中国石油化工股份有限公司 | Preparation method of nanometer silicon hydroxide-aluminum hydroxide powder |
| CN102451673A (en) * | 2010-10-15 | 2012-05-16 | 中国石油化工股份有限公司 | Preparation method of nanometer silicon hydroxide-aluminum hydroxide powder |
| CN104341568B (en) * | 2013-07-26 | 2018-11-02 | 五邑大学 | A kind of preparation method of nano silicon dioxide polyethers (ester) polyol dispersions of modified polyurethane |
| CN104341568A (en) * | 2013-07-26 | 2015-02-11 | 五邑大学 | Preparation method of nanometer silica polyether (ester) polyol dispersion for modifying polyurethane |
| CN103449454B (en) * | 2013-09-18 | 2015-12-23 | 武汉科技大学 | A kind of is that raw material prepares the method for nano silicon and preparation-obtained nano silicon with the leaf of bamboo |
| CN103449454A (en) * | 2013-09-18 | 2013-12-18 | 武汉科技大学 | Method for preparing nano silicon dioxide by using bamboo leaves as materials and nano silicon dioxide prepared by method |
| CN104030302A (en) * | 2014-06-16 | 2014-09-10 | 深圳迈思瑞尔科技有限公司 | Method for preparing silicon dioxide pellets |
| CN104556076A (en) * | 2015-02-03 | 2015-04-29 | 苏州纳迪微电子有限公司 | Preparation method of ultrahigh-purity amorphous spherical silica powder |
| CN104891506A (en) * | 2015-06-05 | 2015-09-09 | 确成硅化学股份有限公司 | Manufacturing method of low-BET high-dispersivity silica white |
| CN105000567A (en) * | 2015-07-30 | 2015-10-28 | 西南石油大学 | Preparation method for high-dispersity nano-silica |
| CN105000567B (en) * | 2015-07-30 | 2017-03-29 | 西南石油大学 | A kind of preparation method of high-dispersion nano silicon dioxide |
| CN106147892A (en) * | 2016-07-26 | 2016-11-23 | 深圳市前海龙达新能源有限公司 | A kind of white oil nanometer additive, preparation method and modified white oil thereof |
| CN106381087A (en) * | 2016-08-27 | 2017-02-08 | 安徽龙泉硅材料有限公司 | Preparation method of precipitated silica for water-based adhesive |
| CN106378056B (en) * | 2016-08-27 | 2018-10-26 | 安徽龙泉硅材料有限公司 | A kind of pigment dispersing agent prepared using parental type precipitated silica |
| CN106378056A (en) * | 2016-08-27 | 2017-02-08 | 安徽龙泉硅材料有限公司 | Pigment dispersing agent prepared by amphiphilic precipitated silica |
| CN108017061A (en) * | 2017-12-06 | 2018-05-11 | 上海应用技术大学 | One kind prepares large-specific surface area nano SiO using waterglass2Method |
| CN108017061B (en) * | 2017-12-06 | 2020-12-08 | 上海应用技术大学 | Method for preparing large-specific-surface-area nano SiO by using water glass2Method (2) |
| CN108069430A (en) * | 2017-12-28 | 2018-05-25 | 无锡恒诚硅业有限公司 | A kind of preparation method of high dispersive precipitated silica and precipitated silica therefrom |
| CN109399639A (en) * | 2018-12-10 | 2019-03-01 | 中国医科大学 | A kind of preparation method of regulation ball shaped nano silicon particle and spherical mesoporous silicon nanoparticle |
| CN113789042A (en) * | 2021-11-03 | 2021-12-14 | 广东特普爱高分子材料有限公司 | Flame-retardant environment-friendly PC-ABS composite plastic master batch and preparation method thereof |
| CN113789042B (en) * | 2021-11-03 | 2023-08-08 | 广东特普爱高分子材料有限公司 | Flame-retardant environment-friendly PC-ABS composite plastic master batch and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100345755C (en) | 2007-10-31 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100345755C (en) | Nano silicon dioxide preparation method | |
| Ezzat et al. | Evaluation of asphalt binders modified with nanoclay and nanosilica | |
| EP1357156B1 (en) | Silane modified oxidic or silicate filler, method for its manufacture and its use | |
| EP2268729B1 (en) | Particulate wax composites having a core/shell structure and method for the production thereof and the use thereof | |
| ATE514654T1 (en) | CATIONICALLY STABILIZED AQUEOUS SILICA DISPERSION, METHOD FOR THE PRODUCTION THEREOF AND THEIR USE. | |
| EP2049603B1 (en) | Surface-modified particles and production method | |
| DE2435860B2 (en) | PROCESS FOR THE PRODUCTION OF FINE PARTICLE HYDROPHOBIC SILICACIDS OR SILICATES | |
| EP3405433B1 (en) | Method for producing modified precipitated silica | |
| EP0126871A1 (en) | Surface-modified natural oxidic or silicic fillers, method for their preparation and their use | |
| CA3017484C (en) | Metal-based hydrogen sulfide scavenger and method of preparing same | |
| WO2004106423A2 (en) | Solvent-containing compositions based on polychloroprene | |
| WO2015091412A1 (en) | Silane-modified silcic acid, method for the production and use thereof | |
| EP2291235A1 (en) | Novel composite materials, method for preparing same and uses thereof | |
| CN104059096B (en) | Small-particle-size oversized-aperture mesopore organic silicon nanometer particles and preparation method thereof | |
| WO2019161912A1 (en) | Highly dispersible precipitated silicas | |
| US7758689B2 (en) | Nano-talc with hydrophobic coating | |
| DE2938074A1 (en) | METHOD FOR REMOVING SULFUR AND ASH FROM COAL | |
| Bakir et al. | Slow settling behaviour of soil nano-particles in water and synthetic sugarcane juice solutions | |
| EP3201132A1 (en) | Method for producing aerogels | |
| US5938832A (en) | Crumb rubber modified asphalt with enhanced settling characteristics | |
| CN112920625A (en) | Modified carbon black and preparation method thereof | |
| CN106147951A (en) | A kind of lubricant oil composite and preparation method thereof | |
| JP2003267722A (en) | Nonporous spherical silica and method of manufacturing it | |
| CN117326564B (en) | Production process of material for enhancing wear resistance of tire | |
| CN109052413A (en) | Preparation method of the size between 20 ~ 50 nanometers of mesoporous silica nanospheres shape particle |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |