CN102020285A - Preparation method for hydrophobic silica aerogel - Google Patents
Preparation method for hydrophobic silica aerogel Download PDFInfo
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Abstract
The present invention discloses a preparation method for hydrophobic silica aerogel with industrial waterglass as a raw material, which comprises the following steps: diluting the industrial waterglass with water; neutralizing with an acid to obtain hydrosol; allowing the hydrosol to stand and age for 8-48 hours at normal temperature so as to form hydrogel; replacing the water in the hydrogel with anhydrous ethanol; allowing the hydrogel to react with organosilane compounds; performing surface modification and simultaneous solvent exchange with n-hexane; suction-filtering; washing; allowing to stand at normal temperature to obtain white hydrophobic silica aerogel powder. The preparation method has simple process and low cost, and the prepared aerogel has porous network-like structure which features a low density and a high specific surface area.
Description
Technical field
The present invention relates to a kind of preparation method of hydrophobic silicon dioxide aerogel, belong to the inorganic porous material technical field.
Background technology
SiO
2Aerogel is a kind of novel light nano-porous materials, and characteristics such as density is low, specific surface area is big, porosity height that it has are a kind of novel nano-materials with broad prospect of application.SiO
2Aerogel has the character of multiple uniqueness, for example low specific refractory power, low Young's modulus, low acoustic impedance, lower thermal conductivity, strong adsorptivity, typical fractal structure etc., can be made into multiple high performance materials such as specific acoustic resistance coupling material, filtering material, high temperature insulating material, be with a wide range of applications.
People adopt supercritical drying to prepare aerogel at first, because it can keep the nano-porous structure of aerogel.But the required plant and instrument complexity of supercritical drying, costliness, and require relatively harsher to the selection of each condition and parameter.Therefore, adopt constant pressure and dry to prepare SiO
2Aerogel is its inevitable requirement of accomplishing scale production and using.Constant pressure and dry technology mainly contains following path: 1) repeatedly exchange of solvent and burin-in process for a long time; 2) add surface-modifying agent and carry out hydrophobic treatment.
In addition, in the process of preparation hydrogel, the material of having reported as the silicon source has positive silicate class (methyl silicate and tetraethoxy), poly silane, silicon sol, water glass, and more cheap rice husk or flyash etc. are as the silicon source.Adopt silicon ester (TEOS, TMOS etc.) can successfully prepare SiO for raw material
2Aerogel costs an arm and a leg problems such as cost height, medicine toxicity but exist.
Adopt service water glass to reduce production costs greatly, employing water glass such as the FeiShi of Dalian University of Technology are the silicon source, adopt ion exchange method to prepare hydrogel, by a step exchange of solvent and a finishing method, the gained hydrogel is soaked in ethanol (EtOH)/trimethylchlorosilane (TMCS)/heptane, synthesized aerosil under the constant pressure and dry.The Shen Jun of Tongji University etc. are the silicon source with the industrial-grade sodium silicate, and water is reactant and solvent, adopt HF one step quick catalysis method and HNO respectively
3-NaOH soda acid two-step catalysis method, go out silica hydrogel by sol-gel technology preparing, adopt trimethylchlorosilane (TMCS) and hexamethyldisiloxane (HMDSO) as coating materials, prepare nano-stephanoporate silicon dioxide under the condition of normal pressure with high-efficiency insulated performance.
Adopting rice husk or flyash is feedstock production SiO
2Aerogel is a kind of approach that reduces cost, saves the energy, all is that the employing rice hull ash is that feedstock production obtains aerosil as Chinese patent CN1449997, CN101244826, CN1669921, CN1724353, CN101259964, CN101348255 etc.The first step of this type of way all is to utilize the highly basic leaching, utilizes effective constituent water glass wherein to carry out the preparation of silicon-dioxide then.
The present invention is a raw material with service water glass, prepares hydrophobic silicon dioxide aerogel by simple sol-gel method, and preparation time is short, and operating procedure is simple.
Summary of the invention
The technical issues that need to address of the present invention are the preparation methods that disclose a kind of hydrophobic silicon dioxide aerogel.
Method of the present invention comprises the steps:
(1) preparation of the water-sol
Under the normal temperature, with service water glass dilute with water, to 5-8, obtain the water-sol with sour adjust pH, wherein used acid is a kind of in hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid or the acetic acid, and wherein acid concentration is 1-5mol/L;
(2) colloidal sol is aging
Under the normal temperature, the water-sol left standstill aging 12-48 hour, formed hydrogel, and distilled water wash is for several times to remove sodium ion;
(3) solvent exchange
Under the normal temperature, hydrogel is immersed in the solvent orange 2 A, displaces water in the gel with solvent orange 2 A, the time is 8-48 hour, and solvent orange 2 A is a kind of in methyl alcohol, ethanol, n-propyl alcohol, Virahol or the acetone;
(4) surface modification/solvent exchange
To be immersed among the solvent B through the gel after the solvent orange 2 A displacement, and react with organic silane compound, carry out surface modification and solvent exchange simultaneously, under the normal temperature modification 8-48 hour, wherein the mol ratio of silicon-dioxide is 0.05-1 in organic silane compound and the gel, organic silane compound is a trimethylchlorosilane, a kind of in dimethyldichlorosilane(DMCS), METHYL TRICHLORO SILANE, chlorotriethyl silane, diethyl dichlorosilane or the ethyl trichlorosilane, solvent B are a kind of in normal hexane, Skellysolve A or the normal heptane;
(5) constant pressure and dry
To leave standstill under the normal temperature and obtain white hydrophobic silicon dioxide aerogel powder through the gel filtering and washing behind surface modification and the solvent exchange.
The present invention compared with prior art has the following advantages:
1, adopting cheap service water glass is raw material, and production cost reduces;
2, adopt solvent exchange and surface modification to realize constant pressure and dry, all processes are all carried out at normal temperatures, and cost reduces;
3, preparation time is shorter, and technology is simple;
4, the aerogel of preparing has low density (0.1-0.18g/cm
3), high specific surface area (500-700m
2/ g), mean pore size is 15-20nm.
Description of drawings
The contact angle figure of accompanying drawing 1 aerosil
The SEM figure of accompanying drawing 2 aerosils
Embodiment
Embodiment 1
Measure 5ml service water glass (modulus is 3.3), the dilution of 30ml deionized water is filtered.The 2mol/L dilute sulphuric acid transfers to pH=7, and room temperature left standstill 12 hours, deionized water wash 4-6 time.25ml soaked in absolute ethyl alcohol 12 hours, suction filtration, absolute ethanol washing twice, 2.5ml trimethylchlorosilane (TMCS) and 25ml normal hexane (n-hexane) soaked 12 hours, suction filtration, normal hexane washing three times, room temperature leaves standstill.
The contact angle figure of Fig. 1 aerosil, about 130 ° of contact angles, the result shows that aerosil is hydrophobic.
Embodiment 2
Measure 10ml service water glass (modulus is 3.3), the dilution of 50ml deionized water is filtered.2mol/L dilute hydrochloric acid transfers to pH=8, and room temperature left standstill 24 hours, deionized water wash 4-6 time.40ml soaked in absolute ethyl alcohol 24 hours, suction filtration, absolute ethanol washing twice, 6ml trimethylchlorosilane (TMCS) and 50ml normal hexane (n-hexane) soaked 24 hours, suction filtration, normal hexane washing three times, room temperature leaves standstill.
The SEM figure of Fig. 2 aerosil, the result shows that aerosil is continuous poriferous network-like structure.
Embodiment 3
Measure 10ml service water glass (modulus is 3.3), the dilution of 50ml deionized water is filtered.The 5mol/L dilute sulphuric acid transfers to pH=7, and room temperature left standstill 12 hours, deionized water wash 4-6 time.The 40ml Virahol soaked 24 hours, suction filtration, and washed with isopropyl alcohol twice, 6ml trimethylchlorosilane (TMCS) and 50ml normal heptane soaked 36 hours, suction filtration, normal heptane washing three times, room temperature leaves standstill.
Claims (10)
1. one kind is the method for feedstock production hydrophobic silicon dioxide aerogel with service water glass, may further comprise the steps:
(1) preparation of the water-sol
Under the normal temperature,, to 5-8, obtain the water-sol with sour adjust pH with service water glass dilute with water;
(2) colloidal sol is aging
Under the normal temperature, the water-sol forms hydrogel leaving standstill aging 12-48 hour, and distilled water wash is for several times to remove sodium ion;
(3) solvent exchange
Under the normal temperature, displace water in the gel with solvent orange 2 A, the time is 8-48 hour;
(4) surface modification/solvent exchange
To rest among the solvent B through solvent orange 2 A displacement back gel, and react with organic silane compound, and carry out surface modification and solvent exchange simultaneously, under the normal temperature modification 8-48 hour, wherein the mol ratio of silicon-dioxide was 0.05-1 in organic silane compound and the gel.
(5) constant pressure and dry
Will be through the gel suction filtration behind surface modification and the solvent exchange, washing is left standstill under the normal temperature, obtains white hydrophobic silicon dioxide aerogel powder.
2. method according to claim 1 is characterized in that: the industrial concentration of sodium silicate of step (1) is 5%-10%, with sour adjust pH to 5-8.
3. method according to claim 1 is characterized in that: the used acid of step (1) is a kind of in hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid or the acetic acid, and wherein acid concentration is 1-5mol/L;
4. method according to claim 1 is characterized in that: the middle water-sol of step (2) leaves standstill aging at normal temperatures, and the time is 8-48 hour.
5. method according to claim 1 is characterized in that: the water-sol is replaced at normal temperatures in the step (3), and time swap is 8-48 hour, and the displacement number of times is 1-3 time.
6. method according to claim 1 is characterized in that: solvent orange 2 A described in the step (3) is a kind of in methyl alcohol, ethanol, n-propyl alcohol, Virahol or the acetone.
7. method according to claim 1 is characterized in that: colloidal sol carries out surface modification and solvent exchange at normal temperatures in the step (4), and the time is 8-48 hour, and the mol ratio of silicon-dioxide is 0.3-1.5 in organic silane compound and the gel.
8. method according to claim 1, it is characterized in that: the described organic silane compound of step (4) is a trimethylchlorosilane, a kind of in dimethyldichlorosilane(DMCS), METHYL TRICHLORO SILANE, chlorotriethyl silane, diethyl dichlorosilane or the ethyl trichlorosilane.
9. method according to claim 1 is characterized in that: the described solvent B of step (4) is a kind of in normal hexane, Skellysolve A or the normal heptane;
10. method according to claim 1 is characterized in that: solvent exchange all adopts the method for immersion in step (3) and (4).
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