CN104261417A - Preparation method of micro-nano hydroxyl magnesium silicate - Google Patents
Preparation method of micro-nano hydroxyl magnesium silicate Download PDFInfo
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- CN104261417A CN104261417A CN201410486425.8A CN201410486425A CN104261417A CN 104261417 A CN104261417 A CN 104261417A CN 201410486425 A CN201410486425 A CN 201410486425A CN 104261417 A CN104261417 A CN 104261417A
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Abstract
The invention provides a preparation method of micro-nano hydroxyl magnesium silicate. The method is capable of producing high-quality micro-nano hydroxyl magnesium silicate powder products in large scale. The method comprises the following steps: preparing sodium hydroxide into a 0.001-2mol/L solution; mixing nanometer magnesia and nanosilicon dioxide in a container according to a mole ratio of 1 to (0.5-2), adding the prepared sodium hydroxide solution into the container, transferring the solution to a reaction kettle, and reacting for 24-96 hours under the condition at the temperature of 170-300 DEG C; filtering the reacted mixture solution by pure water and drying the filter cake after filtering under the condition at the temperature of 50-100 DEG C to obtain the micro-nano hydroxyl magnesium silicate powder. According to the method, by virtue of precursor nanometer magnesia and nanosilicon dioxide, the micro-nano hydroxyl magnesium silicate is synthesized by a high-temperature hydrothermal method under the condition of a strong base; the thickness of hydroxyl magnesium silicate powder pieces is between 60 nanometers and 20 microns.
Description
Technical field
The present invention relates to micro/nano level raw powder's production technology, particularly a kind of preparation method of micro/nano level hydroxyl magnesium silicate.
Background technology
The application of hydroxyl magnesium silicate is very extensive.The main source of current hydroxyl magnesium silicate carries out mechanical disintegration to natural silicate ore to obtain, and its impurity is many, not easily purify, diameter of particle is uneven, and consistence difference is difficult to reach nano level.The shortcoming of natural crystal makes it apply and receives very big restriction.The development of nanotechnology makes to prepare micro/nano level hydroxyl magnesium silicate becomes possibility.Open (bulletin) number: the CN101386713A of patent, disclose a kind of nano hydroxyl magnesium silicate powder and preparation method thereof, the method adopts diatomite, magnesium sulfate, sodium hydroxide, sodium peroxide to be the synthesis that raw material carries out hydroxyl magnesium silicate.The shortcoming of the method is that the consistence of the sample of synthesis is difficult to control.
Summary of the invention
The invention provides a kind of preparation method of micro/nano level hydroxyl magnesium silicate, large-scale production high-quality micro/nano level hydroxyl magnesium silicate powder product.
A preparation method for micro/nano level hydroxyl magnesium silicate, the method comprises the following steps:
A. sodium hydroxide is made into the solution of 0.001 ~ 2mol/L;
B. nano magnesia and nano silicon are mixed in a reservoir according to the ratio that mol ratio is 1: 0.5 ~ 2, add the sodium hydroxide solution prepared in step a in a reservoir, add-on is 50% ~ 99% of container volume, after fully mixing in a reservoir, move in reactor, be under the condition of 170 DEG C ~ 300 DEG C in temperature, reaction 24h ~ 96h;
C. adopt pure water to be filtered by reacted mixing solutions, until filtrate is in neutral, by dry under the condition of 50 DEG C ~ 100 DEG C for the filter cake after filtering, obtain micro/nano level hydroxyl magnesium silicate powder.
The present invention is compared with similar technique, and its significant beneficial effect is embodied in:
The present invention utilizes presoma nano magnesia and nano silicon, utilizes high temperature hydrothermal method synthetizing micro-nano level hydroxyl magnesium silicate when highly basic.Nano silicon and nano magnesia are high purity and highly active micro/nano level powder, and hydroxyl magnesium silicate powder sheet becomes thickness 60nm ~ 20um.
Accompanying drawing explanation
Fig. 1 is the surface sweeping electron microscopic picture of embodiment 1 micro/nano level hydroxyl magnesium silicate powder surface topography.
Fig. 2 is the surface sweeping electron microscopic picture of embodiment 2 micro/nano level hydroxyl magnesium silicate powder surface topography.
Fig. 3 is the surface sweeping electron microscopic picture of embodiment 3 micro/nano level hydroxyl magnesium silicate powder surface topography.
Fig. 4 is the surface sweeping electron microscopic picture of embodiment 4 micro/nano level hydroxyl magnesium silicate powder surface topography.
Fig. 5 is the surface sweeping electron microscopic picture of embodiment 5 micro/nano level hydroxyl magnesium silicate powder surface topography.
Fig. 6 is embodiment 1 micro/nano level hydroxyl magnesium silicate powder x-ray diffracting spectrum.
Fig. 7 is embodiment 2 micro/nano level hydroxyl magnesium silicate powder x-ray diffracting spectrum.
Fig. 8 is embodiment 3 micro/nano level hydroxyl magnesium silicate powder x-ray diffracting spectrum.
Fig. 9 is embodiment 4 micro/nano level hydroxyl magnesium silicate powder x-ray diffracting spectrum.
Figure 10 is embodiment 5 micro/nano level hydroxyl magnesium silicate powder x-ray diffracting spectrum.
Embodiment
The present invention is described in more detail below by embodiment.
Embodiment 1
The step of a kind of preparation method of micro/nano level hydroxyl magnesium silicate:
A. sodium hydroxide is mixed with the aqueous solution of 1mol/L;
B. nano magnesia and nano silicon are mixed in a reservoir according to the ratio that mol ratio is 3: 2, and add the sodium hydroxide solution of step a preparation, add-on is 80% of container volume.Moving into reactor after abundant mixing, is react 72h under the condition of 200 DEG C in temperature;
C. adopt pure water to be filtered by reacted mixing solutions, until filtrate is in neutral, by dry under the condition of 80 DEG C for the filter cake after filtering, obtain micro/nano level hydroxyl magnesium silicate powder.
Product performance detect:
XRD and TEM (transmission electron microscope) analysis detected result are carried out as shown in Fig. 1 (SEM), Fig. 6 (XRD) to obtained micro/nano level hydroxyl magnesium silicate powder.
Embodiment 2
The step of a kind of preparation method of micro/nano level hydroxyl magnesium silicate:
A. sodium hydroxide is mixed with the aqueous solution of 0.5mol/L;
B. nano magnesia and nano silicon are mixed in a reservoir according to the ratio that mol ratio is 1: 1, and add the sodium hydroxide solution of step a preparation, add-on is 60% of container volume.Moving into reactor after abundant mixing, is react 96h under the condition of 180 DEG C in temperature;
C. adopt pure water to be filtered by reacted mixing solutions, until filtrate is in neutral, by dry under the condition of 80 DEG C for the filter cake after filtering, finally make micro/nano level hydroxyl magnesium silicate powder.
Product performance detect:
XRD and TEM (transmission electron microscope) analysis detected result are carried out as shown in Fig. 2 (SEM), Fig. 7 (XRD) to obtained nano-grade hydroxy magnesium silicate powder.
Embodiment 3
The step of a kind of preparation method of micro/nano level hydroxyl magnesium silicate:
A. sodium hydroxide is mixed with the aqueous solution of 2mol/L;
B. nano magnesia and nano silicon are mixed in a reservoir according to the ratio that mol ratio is 4: 3, and add the sodium hydroxide solution of step a preparation, add-on is 90% of container volume.Moving into reactor after abundant mixing, is react 48h under the condition of 220 DEG C in temperature;
C. adopt pure water to be filtered by reacted mixing solutions, until filtrate is in neutral, by dry under the condition of 80 DEG C for the filter cake after filtering, finally make micro/nano level hydroxyl magnesium silicate powder.
Product performance detect:
XRD and TEM (transmission electron microscope) analysis detected result are carried out as shown in Fig. 3 (SEM), Fig. 8 (XRD) to obtained nano-grade hydroxy magnesium silicate powder.
Embodiment 4
The step of a kind of preparation method of micro/nano level hydroxyl magnesium silicate:
A. sodium hydroxide is mixed with the aqueous solution of 0.1mol/L;
B. nano magnesia and nano silicon are mixed in a reservoir according to the ratio that mol ratio is 3: 2, and add the sodium hydroxide solution of step a preparation, add-on is 70% of container volume.Moving into reactor after abundant mixing, is react 36h under the condition of 250 DEG C in temperature;
C. adopt pure water to be filtered by reacted mixing solutions, until filtrate is in neutral, by dry under the condition of 80 DEG C for the filter cake after filtering, finally make micro/nano level hydroxyl magnesium silicate powder.
Product performance detect:
XRD and TEM (transmission electron microscope) analysis detected result are carried out as shown in Fig. 4 (SEM), Fig. 9 (XRD) to obtained nano-grade hydroxy magnesium silicate powder.
Embodiment 5
The step of a kind of preparation method of micro/nano level hydroxyl magnesium silicate:
A. sodium hydroxide is mixed with the aqueous solution of 0.1mol/L;
B. nano magnesia and nano silicon are mixed in a reservoir according to the ratio that mol ratio is 2: 1, and add the sodium hydroxide solution of step a preparation, add-on is 70% of container volume.Moving into reactor after abundant mixing, is react 24h under the condition of 270 DEG C in temperature;
C. adopt pure water to be filtered by reacted mixing solutions, until filtrate is in neutral, by dry under the condition of 80 DEG C for the filter cake after filtering, finally make micro/nano level hydroxyl magnesium silicate powder.
Product performance detect:
XRD and TEM (transmission electron microscope) analysis detected result are carried out as shown in Fig. 5 (SEM), Figure 10 (XRD) to obtained nano-grade hydroxy magnesium silicate powder.
Claims (1)
1. a preparation method for micro/nano level hydroxyl magnesium silicate, is characterized in that the method comprises the following steps:
A. sodium hydroxide is made into the solution of 0.001 ~ 2mol/L;
B. nano magnesia and nano silicon are mixed in a reservoir according to the ratio that mol ratio is 1: 0.5 ~ 2, add the sodium hydroxide solution prepared in step a in a reservoir, add-on is 50% ~ 99% of container volume, after fully mixing in a reservoir, move in reactor, be under the condition of 170 DEG C ~ 300 DEG C in temperature, reaction 24h ~ 96h;
C. adopt pure water to be filtered by reacted mixing solutions, until filtrate is in neutral, by dry under the condition of 50 DEG C ~ 100 DEG C for the filter cake after filtering, obtain micro/nano level hydroxyl magnesium silicate powder.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105152178A (en) * | 2015-07-13 | 2015-12-16 | 北京交通大学 | Preparation method of nanometer magnesium silicate hydroxide, and preparation method and application of anti-wear agent |
| CN106966401A (en) * | 2017-03-24 | 2017-07-21 | 清华大学 | Oil solubility nanometer hydroxyl magnesium silicate and preparation method thereof |
| CN107500303A (en) * | 2017-08-14 | 2017-12-22 | 曲阜师范大学 | A kind of mesoporous magnesium silicate microballoon and its hydro-thermal thermal transition preparation method |
| CN110305714A (en) * | 2019-06-26 | 2019-10-08 | 北京交通大学 | Nano hydroxyl magnesium silicate-Fluorin doped agraphitic carbon antiwear composite agent preparation method |
| CN111100723A (en) * | 2019-03-27 | 2020-05-05 | 南京金魔节能工程有限公司 | Preparation method of metal friction pair rapid wear-resistant repair material |
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| CN101386713A (en) * | 2008-07-28 | 2009-03-18 | 中国人民解放军装甲兵工程学院 | Nano hydroxyl magnesium silicate powder and preparation method thereof |
| CN103880027A (en) * | 2014-04-10 | 2014-06-25 | 周璐 | Hydroxyl magnesium silicate nanotube wear-resistant material and preparation method thereof |
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2014
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101386713A (en) * | 2008-07-28 | 2009-03-18 | 中国人民解放军装甲兵工程学院 | Nano hydroxyl magnesium silicate powder and preparation method thereof |
| CN103880027A (en) * | 2014-04-10 | 2014-06-25 | 周璐 | Hydroxyl magnesium silicate nanotube wear-resistant material and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105152178A (en) * | 2015-07-13 | 2015-12-16 | 北京交通大学 | Preparation method of nanometer magnesium silicate hydroxide, and preparation method and application of anti-wear agent |
| CN105152178B (en) * | 2015-07-13 | 2017-12-22 | 北京交通大学 | The preparation method of nano hydroxyl magnesium silicate, the preparation method and application of antiwear additive |
| CN106966401A (en) * | 2017-03-24 | 2017-07-21 | 清华大学 | Oil solubility nanometer hydroxyl magnesium silicate and preparation method thereof |
| CN106966401B (en) * | 2017-03-24 | 2019-02-05 | 清华大学 | Oil solubility nanometer hydroxyl magnesium silicate and preparation method thereof |
| CN107500303A (en) * | 2017-08-14 | 2017-12-22 | 曲阜师范大学 | A kind of mesoporous magnesium silicate microballoon and its hydro-thermal thermal transition preparation method |
| CN107500303B (en) * | 2017-08-14 | 2019-10-08 | 曲阜师范大学 | A kind of mesoporous magnesium silicate microballoon and its hydro-thermal-thermal transition preparation method |
| CN111100723A (en) * | 2019-03-27 | 2020-05-05 | 南京金魔节能工程有限公司 | Preparation method of metal friction pair rapid wear-resistant repair material |
| CN111100723B (en) * | 2019-03-27 | 2023-08-22 | 南京金魔节能工程有限公司 | Preparation method of rapid wear-resistant repair material for metal friction pair |
| CN110305714A (en) * | 2019-06-26 | 2019-10-08 | 北京交通大学 | Nano hydroxyl magnesium silicate-Fluorin doped agraphitic carbon antiwear composite agent preparation method |
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