Method for preparing flaky silicic acid zirconium nanocrystalline

A technology of zirconium silicate and nanocrystals, applied in nanotechnology, chemical instruments and methods, silicon compounds, etc., can solve the problems of high preparation temperature and short preparation time, and achieve low reaction temperature, short cycle and narrow particle size distribution Effect

Active Publication Date: 2013-04-10
临沂市高新汽车租赁服务有限公司
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  • Claims
  • Application Information

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Problems solved by technology

Jiang Weihui et al. (Chinese patent 200710108375.X) used commercially pure anhydrous zirconium tetrachloride and ethyl orthosilicate as precursors, and synthesized it by non-hydrolytic sol-gel method at 700°C for 15 minutes by selecting a suitable mineralizer. Zirconium silicate powder, although the preparation time of this method is short, the preparation temperature is relatively high

Method used

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  • Method for preparing flaky silicic acid zirconium nanocrystalline

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] 1) Separately analyze pure ZrCl 4 , ethyl orthosilicate (CH 3 CH 2 OSi(OCH 2 CH 3 ) 3 ), cetyltrimethylammonium bromide (CTAB) was added into distilled water and stirred to make ZrCl 4 The molar concentration of the precursor solution A is 1.0mol / L, where ZrCl 4 :CH 3 CH 2 OSi(OCH 2 CH 3 ) 3 : The molar ratio of CTAB is 2: 1: 6;

[0017] 2) Add hydrochloric acid dropwise to the precursor solution A to adjust the pH value to 1.5, and keep stirring to form sol B, and then age sol B at room temperature for 24 hours to obtain gel D;

[0018] 3) Put the gel D into a constant temperature drying oven to dry at 100°C, and put it into a mortar to grind after drying to obtain a powder E;

[0019] 4) Prepare the powder E into a suspension with a solid content of 20g / L, then pour the suspension into a hydrothermal reaction kettle, and control the filling ratio at 40%; then seal the hydrothermal kettle and put it into a microwave water reactor React at 280°C for 30 minu...

Embodiment 2

[0022] 1) Separately analyze pure ZrCl 4 , ethyl orthosilicate (CH 3 CH 2 OSi(OCH 2 CH 3 ) 3 ), cetyltrimethylammonium bromide (CTAB) was added into distilled water and stirred to make ZrCl 4 The molar concentration of the precursor solution A is 0.7mol / L, where ZrCl 4 :CH 3 CH 2 OSi(OCH 2 CH 3 ) 3 : The molar ratio of CTAB is 4: 3: 4;

[0023] 2) Add hydrochloric acid dropwise to the precursor solution A to adjust the pH value to 3.5, and keep stirring to form sol B, and then age sol B at room temperature for 36 hours to obtain gel D;

[0024] 3) Put the gel D in a constant temperature drying oven to dry at 150°C, and put it into a mortar to grind after drying to obtain the powder E;

[0025] 4) Prepare the powder E into a suspension with a solid content of 5g / L, then pour the suspension into a hydrothermal reaction kettle, and control the filling ratio at 60%; then seal the hydrothermal kettle, and put it into the microwave water React at 240°C for 45 minutes in...

Embodiment 3

[0028] 1) Separately analyze pure ZrCl 4 , ethyl orthosilicate (CH 3 CH 2 OSi(OCH 2 CH 3 ) 3 ), cetyltrimethylammonium bromide (CTAB) was added into distilled water and stirred to make ZrCl 4 The molar concentration of the precursor solution A is 0.9mol / L, where ZrCl 4 :CH 3 CH 2 OSi(OCH 2 CH 3 ) 3 : The molar ratio of CTAB is 7: 5: 2;

[0029] 2) Add hydrochloric acid dropwise to the precursor solution A to adjust the pH to 5, and keep stirring to form sol B, and then age sol B at room temperature for 72 hours to obtain gel D;

[0030] 3) Put the gel D into a constant temperature drying oven to dry at 200°C, and put it into a mortar for grinding after drying to obtain powder E;

[0031] 4) Prepare the powder E into a suspension with a solid content of 30g / L, then pour the suspension into a hydrothermal reaction kettle, and control the filling ratio at 80%; then seal the hydrothermal kettle, and put it into the microwave water React at 200°C for 60 minutes in a th...

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Abstract

The invention discloses a method for preparing flaky silicic acid zirconium nanocrystalline. ZrCl4, ethyl orthosilicate and CTAB are added into distilled water for obtaining a precursor liquid A, hydrochloric acid is added into the precursor liquid A to adjust the PH value to be 1 to 5, and a gelatin D is obtained at the room temperature through ageing; the gelatin D is put into a constant temperature drying box for drying, and then put into a mortar box for grinding after being dried, and powder E is obtained; the power E is prepared into a suspending liquid, then the suspending liquid is poured into a hydrothermal reaction kettle, then the hydrothermal reaction kettle is sealed and placed into a microwave hydrothermal reaction instrument for reaction, after reaction, and then through natural cooling to the room temperature, a cooling solution F is obtained; the solution F is collected through suction filtration of filter paper, then both deionized water and absolute ethyl alcohol are adopted for washing, and then the flaky silicic acid zirconium nanocrystalline is obtained through drying in an electric heating blast drying box. In the invention, sol-gel is adopted for assisting a microwave hydrothermal method to prepare the flaky silicic acid zirconium nanocrystalline, since the reaction is accomplished in liquid phase, later annealing crystallization treatment is not required, the particle size distribution of obtained silicic acid zirconium nanocrystalline is narrow, the crystal formation is controllable, the reaction temperature is low, the period is short, and the repetitiveness is excellent.

Description

technical field [0001] The invention belongs to the field of material chemical industry, and in particular relates to a method for preparing sheet zirconium silicate nanocrystals by a sol-gel assisted microwave hydrothermal method. Background technique [0002] Zirconium silicate (ZrSiO 4 ) belongs to the tetragonal crystal system and is a silicate mineral with an island structure. Zirconium silicate can be used as a high-performance structural material (such as graphite, C / C composite materials and SiC structural ceramics, etc.) due to its high melting point, low thermal conductivity, low expansion coefficient, and excellent chemical and phase stability. High temperature oxidation resistant coating material. [0003] At present, the methods for preparing zirconium silicate crystals mainly include solid-state reaction method, precipitation method, hydrothermal method, and sol-gel method. The above methods generally require high temperature (such as 1300-1600°C for solid-s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/20B82Y40/00
Inventor 曹丽云刘佳侯艳超黄剑锋吴建鹏辛宇
Owner 临沂市高新汽车租赁服务有限公司
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