Preparation method of hydrophobic lipophilic sponge aerogel composite material

A hydrophobic, lipophilic and composite material technology, applied in the field of porous materials, can solve the problems of long preparation cycle, low compressive strength, gel structure damage, etc., and achieve easy portability and transportation, enhanced mechanical strength, and less organic solvent. Effect

Inactive Publication Date: 2015-09-23
HEFEI KESIFU SAFETY TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the material has poor mechanical properties and is brittle, which limits its application
The "Preparation and Characterization of Flexible Block Hydrophobic Silica Airgel" reported in "Journal of Silicates" all use methyltrimethoxysilane as the precursor, and the wet gel is prepared by the sol-gel method. , solvent exchange and other steps, and dry under normal pressure to prepare silica airgel with certain flexibility, but the preparation process is relatively complicated and the preparation cycle is long
"Microporous and Mesoporous Materials" (MICROPOROUS AND MESOPOROUS MATERIALS, 2012, 148:152-158) reported the stress-strain curve of the flexible aerogel based on methyltrimethoxysilane, indicating that the material is resistant to The compressive strength is very low. When it is compressed by 60%, the required stress is only 22kPa, and it is fragile, so it is not suitable for transportation and carrying
[0003] About adopting sponge to strengthen the report, a kind of preparation method of low-density SiO2 airgel / sponge composite material, adopt two-step sol-gel method to combine CO2 supercritical drying to prepare low-density SiO2 airgel / sponge composite material, adopted The silicon source is methyl orthosilicate, ethyl orthosilicate, water glass or silica sol, and supercritical drying is used, which consumes a lot of energy and costs high, and the final airgel is hydrophilic, so its application is limited. The preparation process is complex (3-8 solvent replacements are required)
A reusable cheap silicon airgel oil-absorbing sponge and its preparation method, using alkoxysilane as a precursor, aging and physical extrusion washing treatment after gelation, the process is relatively complicated, and the extrusion washing scale is difficult to control, Easy to damage the gel structure
Although the final gel has a certain degree of elasticity, the adsorbed organic solvent or oil can be recovered by physical extrusion, but the efficiency of this extrusion recovery method is too low, and it is unlikely in the case of a large amount of fuel oil leakage Effectively stop the flow of oil pollution and pollution behavior
The prior art also discloses a method for hydrophobic and lipophilic treatment of sponges. The cost of the precursor solution and nano-hydrophobic silica particles used is high, and the treatment of the sponge is uneven, and some pores may be blocked.

Method used

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  • Preparation method of hydrophobic lipophilic sponge aerogel composite material
  • Preparation method of hydrophobic lipophilic sponge aerogel composite material
  • Preparation method of hydrophobic lipophilic sponge aerogel composite material

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Experimental program
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Effect test

Embodiment 1

[0030] The specific operation steps for preparing hydrophobic and lipophilic sponge airgel composites are as follows:

[0031] 1. Mix 10ml of methyltrimethoxysilane with 20ml of ethanol, and add 50ml of deionized water (the molar ratio of the three is 1:2.45:15.84) for stirring to form a silicon source solution.

[0032] 2. Add 0.1mol / L hydrochloric acid to the silicon source solution to adjust the pH value of the solution to about 3.6, then add 0.1g F127, stir at room temperature for 20 minutes, add concentrated ammonia water with a concentration of 10mol / L and stir to obtain a pH value of about 8 silica sol.

[0033] 3. Pour the silica sol into a container containing a polyurethane sponge block (3cm×3cm×3cm), and let it stand for 2 hours to form a wet gel.

[0034] 4. Put the wet gel in a drying oven at 100°C and dry it under normal pressure for 6 hours to obtain a hydrophobic and adsorbable sponge-silica airgel composite material with a density of 0.114 g / cm3, a porosity o...

Embodiment 2

[0036] The specific operation steps for preparing hydrophobic and lipophilic sponge airgel composites are as follows:

[0037] 1. Mix 10ml of methyltriethoxysilane with 12.7ml of methanol and add 18.1ml of deionized water (the molar ratio of the three is 1:4.9:15.84) for stirring to form a silicon source solution;

[0038] 2. Add ammonium fluoride with a concentration of 0.5mol / L to the silicon source solution to adjust the pH value of the solution to about 3.8; after stirring at room temperature for 20 minutes, add concentrated ammonia water with a concentration of 5mol / L and stir to obtain silicon with a pH value of about 8. Sol;

[0039] 3. Pour the silica sol into a container containing a polyurethane sponge block (3cm×3cm×3cm), and let it stand for 2 hours to form a wet gel;

[0040]4. Put the wet gel in a drying oven at 80°C and dry it under normal pressure for 8 hours to obtain a hydrophobic and adsorbable sponge-silica airgel composite material with a density of 0.102...

Embodiment 3

[0042] The specific operation steps for preparing hydrophobic and lipophilic sponge airgel composites are as follows:

[0043] 1. Mix 10ml of ethyltriethoxysilane with 17.4ml of isopropanol and add 13.2ml of deionized water (the molar ratio of the three is 1:4.9:15.84) for stirring to form a silicon source solution;

[0044] 2. Add 0.1mol / L hydrochloric acid to the silicon source solution to adjust the pH value of the solution to about 4; then add 0.1g F127, stir at room temperature for 20 minutes, then add concentrated ammonia water with a concentration of 10mol / L and stir to obtain a pH value of about 8 silica sol;

[0045] 3. Pour the silica sol into a container containing a polyurethane sponge block (3cm×3cm×3cm), and let it stand for 6 hours to form a wet gel;

[0046] 4. Put the wet gel in a drying oven at 100°C and dry it under normal pressure for 6 hours to obtain a hydrophobic and adsorbable sponge-silica airgel composite material with a density of 0.121g / cm3, a poro...

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Abstract

The invention discloses a hydrophobic lipophilic sponge aerogel composite material. The composite material is a porous hydrophobic lipophilic solid with compressive strength higher than 0.1MPa, density of 0.09-0.12g/cm<3>, porosity of 90-95%, pore size of 1-10mum, and organic liquid absorption capacity higher than 0.7ml/cm<3>. The preparation method comprises 4 steps: (1) a silicon source and a solvent are mixed; deionized water is added; and the mixture is stirred such that a silicon source solution is formed; (2) an acidic catalyst is added into the silicon source solution for regulating the pH value of the solution; a hydrolysis accelerator is added and the mixture is stirred; an alkaline catalyst is added and the mixture is stirred, such that silica sol is obtained; (3) the silica sol is added into a container containing sponge blocksn, and is allowed to stand, such that wet gel is formed; and (4) the wet gel is dried under normal pressure, such that the hydrophobic lipophilic sponge aerogel composite material is obtained. The preparation method provided by the invention is simple; a preparation period is short, and the entire preparation process can be completed within 12h; steps such as gel aging and solvent exchange are not needed; and a preparation success rate is higher than 98%.

Description

technical field [0001] The invention belongs to the technical field of porous materials, and in particular relates to a preparation method of a sponge airgel porous material. Background technique [0002] Silica airgel is a porous material with low density. After treatment, the material has excellent hydrophobic and lipophilic properties, and can absorb floating oil in water. However, the material has poor mechanical properties and is brittle, which limits its application. The "Preparation and Characterization of Flexible Block Hydrophobic Silica Airgel" reported in "Journal of Silicates" all use methyltrimethoxysilane as the precursor, and the wet gel is prepared by the sol-gel method. , solvent exchange and other steps, followed by normal pressure drying to prepare silica airgel with certain flexibility, but the preparation process is relatively complicated and the preparation cycle is long. "Microporous and Mesoporous Materials" (MICROPOROUS AND MESOPOROUS MATERIALS, 20...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/26B01J20/28B01J20/30C02F1/28
Inventor 何松李治石小靖程旭东陆松
Owner HEFEI KESIFU SAFETY TECH
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