US2009123985A1PendingUtilityA1

Method for fabricating aerogels and their application in biocomposites

Assignee: UNIV CHUNG YUAN CHRISTIANPriority: Nov 10, 2007Filed: Nov 10, 2007Published: May 14, 2009
Est. expiryNov 10, 2027(~1.3 yrs left)· nominal 20-yr term from priority
C01B 33/1585C07D 233/58C12N 11/14C07D 233/56
52
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Claims

Abstract

The present invention discloses a method for fabricating aerogels, a method for fabricating surface-modified aerogels, and a method for fabricating biocomposites. Take the fabricating method of biocomposites for example, first, a precursor solution is provided and the precursor solution comprises a hydrophilic ionic liquid, a catalyzed hydrolysis and/or condensation reagent, at least one biomolecule. Next, a curing process is performed for the precursor solution to hydrolyze and polymerize the at least one alkoxide monomer and/or aryloxide monomer to wrap at least one biomolecule and thus form biocomposite. Afterwards, an extracting process is performed by a solvent for the biocomposite to substitute the ionic liquid in the biocomposite. Finally, a drying process for the biocomposite is carried out after the extracting process so as to remove the solvent in the biocomposite. Therefore, the biocomposite is formed.

Claims

exact text as granted — not AI-modified
1 . A method for fabricating an aerogel, comprising:
 providing an precursor solution comprising an ionic liquid, a catalyzed hydrolysis and/or condensation reagent, and at least one alkoxide monomer and/or aryloxide monomer, where said catalyzed hydrolysis and/or condensation reagent comprises one selected from the group consisting of the following or any combination of the following: alcohol, acidic compound, and alkaline compound;   performing a blending process for said precursor solution to hydrolyze and polymerize said at least one alkoxide monomer and/or aryloxide monomer until the viscosity of said precursor solution reaches a specific viscosity more than or equal to 150 cps;   setting said precursor solution to have said at least one alkoxide monomer and/or aryloxide monomer continue to undergo hydrolysis and condensation, so as to form said aerogel; and   performing an extracting process by a solvent for said aerogel to substitute the ionic liquid in pores of said aerogel.   
   
   
       2 . The method according to  claim 1 , wherein the central element of said alkoxide monomer and/or aryloxide monomer comprises one selected from the group consisting of the following: Li, Na, K, Rb, Cs, Be, Mg, Ca, Sr, Ba, Ti, Te, Cr, Cu, Er, Fe, Ta, V, Zn, Zr, Al, Si, Ge, Sn, and Pb. 
   
   
       3 . The method according to  claim 1 , wherein said alkoxide monomer and/or aryloxide monomer comprises one selected from the group consisting of the following: tetramethyl orthosilicate (TMOS), tetraethoxy orthosilicate (TEOS), bis(triethoxysilyl)ethane (BTSE), bis(triethoxysilyl)benzene (BTSB), tetrabutyl titanate (TBOT), and vanadium oxytriproposide. 
   
   
       4 . The method according to  claim 1 , wherein said ionic liquid is a room temperature ionic liquid. 
   
   
       5 . The method according to  claim 1 , wherein said ionic liquid is formed by mixing an organic base with a Lewis acid that is not halogenated metal acid. 
   
   
       6 . The method according to  claim 5 , wherein the cationic moiety in said organic base is alkyl or aryl group having the following general equation: 
     
       
         
         
             
             
         
       
     
     in which R 1 , R 2 , R 3 , and R 4  are selected according to the following table. 
     
       
         
               
               
               
               
               
             
                   
                   
               
                   
                 R 1   
                 R 2   
                 R 3   
                 R 4   
               
                   
                   
               
                   
                 CH 3   
                 H 
                 CH 3   
                 H 
               
                   
                 C 2 H 5   
                 H 
                 CH 3   
                 H 
               
                   
                 C 2 H 5   
                 H 
                 C 2 H 5   
                 H 
               
                   
                 CH 3 CH 2 CH 2 CH 2   
                 H 
                 CH 3   
                 H 
               
                   
                 (CH 3 ) 2 CHCH 2   
                 H 
                 CH 3   
                 H 
               
                   
                 CH 3 CH 2 CH 2 CH 2   
                 H 
                 C 2 H 5   
                 H 
               
                   
                 CH 3   
                 H 
                 CH 3 OCH 2 CH 2   
                 H 
               
                   
                 CH 3   
                 H 
                 CF 3 CH 2   
                 H 
               
                   
                 CH 3   
                 CH 3   
                 C 2 H 5   
                 H 
               
                   
                 CH 3   
                 CH 3   
                 CH 3 CH 2 CH 2   
                 H 
               
                   
                 C 6 H 6 CH 2   
                 CH 3   
                 CH 3 CH 2 CH 2   
                 H 
               
                   
                 C 6 H 6 CH 2   
                 CH 3   
                 CH 3 CH 2 CH 2 CH 2   
                 H 
               
                   
                 C 6 H 6 CH 2   
                 CH 3   
                 (CH 3 CH 2 )(CH 3 )CH 
                 H 
               
                   
                 C 6 H 6 CH 2   
                 CH 3   
                 CH 3 CH 2 CH 2 CH 2 CH 2   
                 H 
               
                   
                 CH 3   
                 H 
                 C 2 H 5   
                 CH 3   
               
                   
                 C 2 H 5   
                 H 
                 C 2 H 5   
                 CH 3   
               
                   
                   
               
           
              
              
              
             
             
              
              
              
              
              
              
              
              
              
              
              
              
              
              
              
              
              
             
          
         
       
     
   
   
       7 . The method according to  claim 5 , wherein the cation of said organic base comprises one selected from the group consisting of the following: 1-n-butyl-3-methylimidazolium (BMI), 1-octanyl-3-methylimidazolium (OMI), 1-dodecanyl-3-methylimidazolium (DMI), and 1-hexadecanyl-3-methylimidazolium (HDMI). 
   
   
       8 . The method according to  claim 5 , wherein the anionic moiety in said Lewis acid comprises one selected from the group consisting of the following: BF 4 —, PF 6 —, AsF 6 —, SbF 6 —, F(HF) n —, CF 3 SO 3 —, CF 3 CF 2 CF 2 CF 2 SO 3 —, (CF 3 SO 2 ) 2 N—, (CF 3 SO 2 ) 3 C—, CF 3 COO—, and CF 3 CF 2 CF 2 COO—. 
   
   
       9 . The method according to  claim 1 , wherein the weight of said ionic liquid is about 10%˜90%. 
   
   
       10 . The method according to  claim 1 , wherein the weight of said ionic liquid is about 20%˜50%. 
   
   
       11 . The method according to  claim 1 , wherein said specific viscosity is more than or equal to 200 cps. 
   
   
       12 . The method according to  claim 1 , wherein said catalyzed hydrolysis and/or condensation reagent comprises alcohols, and said blending process comprises a heating process. 
   
   
       13 . The method according to  claim 12 , wherein the temperature of said heating process ranges from 50° C. to 150° C. 
   
   
       14 . The method according to  claim 1 , wherein the boiling point of said solvent is less than or equal to 200° C. 
   
   
       15 . The method according to  claim 1 , wherein said solvent comprises one selected from the group consisting of the following: nitrile, alcohol, ketone, and water. 
   
   
       16 . The method according to  claim 1 , wherein the temperature of said extracting process ranges from 50° C. to 200° C. 
   
   
       17 . The method according to  claim 1 , wherein a drying process is carried out after said extracting process, so as to remove the solvent in the pores of said aerogel. 
   
   
       18 . The method according to  claim 1 , wherein said precursor solution further comprises an alkoxide monomer and/or aryloxide monomer with at least one specific moiety, and said specific moiety comprises one selected from the group consisting of the following: carboxyl group, mercapto group, amino group, diamino group, alkyl group, aryl group, epoxy group, and cyano group, so as to form surface-modified aerogel. 
   
   
       19 . The method according to  claim 1 , wherein the composition of said aerogel comprises one selected from the group consisting of the following or any combination of the following: SiO 2 , TiO 2 , V 2 O 5 , and Al 2 O 3 . 
   
   
       20 . The method according to  claim 1 , wherein said aerogel is SiO 2 —TiO 2  two-component aerogel, and the molar ratio of SiO 2  to TiO 2  ranges from 1:9 to 5:5. 
   
   
       21 . The method according to  claim 1 , wherein the specific surface area of said aerogel is more than or equal to 100 m 2 /g. 
   
   
       22 . The method according to  claim 1 , wherein the average pore diameter of said aerogel ranges about 1 nm to 50 nm. 
   
   
       23 . The method according to  claim 1 , wherein the porosity of said aerogel ranges about 50% to 99%. 
   
   
       24 . The method according to  claim 1 , wherein the pore volume of said aerogel is more than or equal to 1.0 cm 3 /g. 
   
   
       25 . A method for fabricating biocomposite, comprising:
 providing a precursor solution comprising a hydrophilic ionic liquid, a catalyzed hydrolysis and/or condensation reagent, and at least one alkoxide monomer and/or aryloxide monomer, wherein said catalyzed hydrolysis and/or condensation reagent comprises one selected from the group consisting of the following or any combination of the following: alcohol and buffer for biomolecules;   performing a curing process for said precursor solution to hydrolyze and polymerize said at least one alkoxide monomer and/or aryloxide monomer to wrap at least one biomolecule and thus form a biocomposite; and   performing an extracting process by a solvent for said biocomposite to substitute the ionic liquid in said biocomposite.   
   
   
       26 . The method according to  claim 25 , wherein said biomolecule comprises one selected from the group consisting of the following: antigens, monoclonal antibodies, polyclonal antibodies, nucleic acids comprising monomeric and oligomeric types, proteins, enzymes, lipids, polysaccharides, sugars, peptides, polypeptides, drugs, viruses, microbes, and bioligands. 
   
   
       27 . The method according to  claim 25 , wherein the central element of said alkoxide monomer and/or aryloxide monomer comprises one selected from the group consisting of the following: Li, Na, K, Rb, Cs, Be, Mg, Ca, Sr, Ba, Ti, Te, Cr, Cu, Er, Fe, Ta, V, Zn, Zr, Al, Si, Ge, Sn, and Pb. 
   
   
       28 . The method according to  claim 25 , wherein said alkoxide monomer and/or aryloxide monomer comprises one selected from the group consisting of the following: tetramethyl orthosilicate (TMOS), tetraethoxy orthosilicate (TEOS), bis(triethoxysilyl)ethane (BTSE), bis(triethoxysilyl)benzene (BTSB), tetrabutyl titanate (TBOT), and vanadium oxytriproposide. 
   
   
       29 . The method according to  claim 25 , wherein said hydrophilic ionic liquid is a room temperature ionic liquid. 
   
   
       30 . The method according to  claim 25 , wherein said hydrophilic ionic liquid is formed by mixing an organic base with a Lewis acid that is not halogenated metal acid. 
   
   
       31 . The method according to  claim 25 , wherein the weight of said hydrophilic ionic liquid is about 10%˜90%. 
   
   
       32 . The method according to  claim 25 , wherein the weight of said hydrophilic ionic liquid is about 20%˜50%. 
   
   
       33 . The method according to  claim 25 , wherein the pH value of said buffer is about 5˜9. 
   
   
       34 . The method according to  claim 25 , wherein said curing process comprises:
 performing a blending process for said precursor solution to hydrolyze and polymerize said at least one alkoxide monomer and/or aryloxide monomer until the viscosity of said precursor solution reaches a specific viscosity that is more than or equal to 150 cps; and   setting said precursor solution to have said at least one alkoxide monomer and/or aryloxide monomer continue to undergo hydrolysis and condensation, so as to form said biocomposite.   
   
   
       35 . The method according to  claim 25 , wherein said specific viscosity is more than or equal to 200 cps. 
   
   
       36 . The method according to  claim 25 , wherein the temperature of said curing process is less than or equal to 50° C. 
   
   
       37 . The method according to  claim 25 , wherein said solvent comprises one selected from the group consisting of the following: alcohol, water, and buffer solution for biomolecules. 
   
   
       38 . The method according to  claim 37 , wherein the pH value of said buffer solution is about 5˜9. 
   
   
       39 . The method according to  claim 25 , wherein the temperature of said extracting process is less than or equal to 50° C. 
   
   
       40 . The method according to  claim 25 , wherein a drying process for said biocomposite is carried out after said extracting process so as to remove the solvent in said biocomposite. 
   
   
       41 . The method according to  claim 40 , wherein the temperature of said drying process is less than or equal to 0° C. 
   
   
       42 . The method according to  claim 40 , wherein the pressure of said drying process is less than or equal to 20 Pa. 
   
   
       43 . The method according to  claim 25 , wherein the specific surface area of said biocomposite is more than or equal to 100 m 2 /g. 
   
   
       44 . The method according to  claim 25 , wherein the average pore diameter of said biocomposite ranges about 1 nm to 50 nm. 
   
   
       45 . The method according to  claim 25 , wherein the porosity of said biocomposite ranges about 50% to 99%. 
   
   
       46 . The method according to  claim 25 , wherein the pore volume of said biocomposite is more than or equal to 1.0 cm 3 /g.

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