Preparation method of porous SiO2 bulk aerogel

A technology of porous silica and gel, which is applied in the field of airgel, can solve the problems of poor weather resistance of organic thermal insulation materials, fire performance that cannot meet the national requirements, and environmental secondary pollution, etc., and achieve excellent thermal insulation performance , Reusable performance improvement, and the effect of improving recyclability

CN107827116AInactive Publication Date: 2018-03-23PAN ASIAN MICROVENT TECH JIANGSU CORP
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Patent Information

Authority / Receiving Office
CN · China
Current Assignee / Owner
Publication Date
2018-03-23
Estimated Expiration
Not applicable · inactive patent

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Abstract

The invention discloses a preparation method of porous SiO2 bulk aerogel, which includes the steps of: A) adding a phase separation agent to a strong acid solution with stirring until the material iscompletely dissolved; B) adding a pore forming agent to the solution in the step A) and fully stirring the solution until complete dissolution; C) adding a silicon source precursor to the solution inthe step B) with stirring until complete hydrolysis; D) adding an accelerant to the solution in the step C) with stirring; E) sealing the sol in the step D) for gelatinization to obtain a product composed of a liquid and gel; F) decanting the liquid in the step E) and adding anhydrous ethanol until the gel is immersed in order to age the gel; G) repeating the step F) to prepare wet gel with anhydrous ethanol replacement; and H) pouring ethanol to the wet gel and increasing pressure in a kettle, heating the kettle and maintaining the temperature, relieving pressure in the kettle, naturally cooling the kettle and opening the high pressure kettle. The aerogel has excellent heat insulation and preservative function and has good repeatability.
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Description

technical field

[0001] The invention relates to the technical field of aerogels, in particular to a method for preparing porous silica block aerogels. Background technique

[0002] At present, the wall thermal insulation materials of domestic buildings are mainly organic polyaniline, polyurethane, etc. Although the thermal insulation performance is excellent, there are also fatal defects. Organic thermal insulation materials have poor weather resistance, especially the fire resistance performance does not meet the national requirements, and poor recycling, easy to cause secondary pollution to the environment, which will bring disastrous consequences after the use of high-rise buildings, in the current organic thermal insulation Under the serious situation of frequent material fires, how to solve the contradiction between the performance of thermal insulation materials, flame retardancy and easy recycling, there is an urgent need for a new type of thermal insulation material ...

Examples

Embodiment 1

[0037] Embodiment 1, refer to Figure 1 to Figure 5

[0038] A kind of preparation method of porous silicon dioxide bulk airgel, is characterized in that, adopts following steps:

[0039] A) Weigh 3.5g of phase separation agent and add it to a concentration of 0.01mol∙L -1 In the nitric acid solution, magnetically stirred until the phase separation agent is completely dissolved, and the phase separation agent is a triblock copolymer polyoxyethylene-polyoxypropylene-polyoxyethylene with an average molecular weight of 5800;

[0040] B) Add 1.0 g of sodium lauryl sulfate pore forming agent to the solution prepared in step A), and stir until the sodium lauryl sulfate pore forming agent is completely dissolved;

[0041] C) Add 2.5 mL of silicon source of tetraethyl orthosilicate precursor to the homogeneous solution obtained in step B), and stir for 3 hours until the silicon source of tetraethyl orthosilicate precursor is completely hydrolyzed;

[0042] D) Add 1.2mL of propylene...

Embodiment 2

[0048] A kind of preparation method of porous silicon dioxide bulk airgel, is characterized in that, adopts following steps:

[0049] A) Weigh 4.0g of phase separation agent and add it to a concentration of 0.05mol∙L -1 In the hydrochloric acid solution, magnetically stirred until the phase separation agent is completely dissolved, and the phase separation agent is a triblock copolymer polyoxyethylene-polyoxypropylene-polyoxyethylene with an average molecular weight of 6500;

[0050] B) Add 0.5 g of 1,3,5-trimethylbenzene pore-forming agent to the solution prepared in step A), and stir well until the 1,3,5-trimethylbenzene pore-forming agent is completely dissolved;

[0051] C) Add 3.5 mL of silicon source of methyl orthosilicate precursor to the homogeneous solution obtained in step B), and stir for 4 hours until the silicon source of methyl orthosilicate precursor is completely hydrolyzed;

[0052] D) Add 2.0mL of propylene oxide or formamide accelerator to the solution obt...

Embodiment 3

[0058] A kind of preparation method of porous silicon dioxide bulk airgel, is characterized in that, adopts following steps:

[0059] A) Weigh 7.0g of phase separation agent and add it to a concentration of 0.1mol∙L -1 In the nitric acid solution, magnetically stirred until the phase separation agent is completely dissolved, and the phase separation agent is a triblock copolymer polyoxyethylene-polyoxypropylene-polyoxyethylene with an average molecular weight of 8400;

[0060] B) Add 2.0 g of sodium lauryl sulfate pore forming agent to the solution prepared in step A), and stir until the sodium lauryl sulfate pore forming agent is completely dissolved;

[0061] C) Add 5.0 mL of silicon source of methyl orthosilicate precursor to the homogeneous solution obtained in step B), and stir for 5 hours until the silicon source of methyl orthosilicate precursor is completely hydrolyzed;

[0062] D) Add 2.5mL of propylene oxide or formamide accelerator to the solution obtained in step ...