Sulfur-containing organic-inorganic hybrid gel compositions and aerogels
View Patent ↗Methods and materials are described for preparing organic-inorganic hybrid gel compositions where a sulfur-containing cross-linking agent covalently links the organic and inorganic components. The gel compositions are further dried to provide porous gel compositions and aerogels. The mechanical and thermal properties of the dried gel compositions are also disclosed.
1. A process comprising the steps of:
providing a sulfur containing cross linking agent;
reacting the sulfur containing cross linking agent with an unsaturated organic polymer to produce a modified organic polymer;
reacting the modified organic polymer with a silica gel precursor to form a modified gel precursor; and
allowing the modified gel precursor to gel to form a gel composition comprising a silica network and the unsaturated organic polymer within the silica network, wherein the unsaturated organic polymer is covalently bound to the silica network through the sulfur containing crosslinking agent.
2. The process of claim 1 further comprising a step of drying the gel composition to produce a porous dry gel composition.
3. The process of claim 1 , wherein the unsaturated organic polymer is selected from the group consisting of unsaturated polyesters; prepolymers based on vinylesters, acrylates, methacrylates, or polyurethanes; polybutadienes; polystyrenes; polyisoprenes; styrene-butadiene copolymers; butadiene-isoprene co-polymers; butadiene-isoprene-styrene terpolymers; copolymers and terpolymers of isobutylene, para-methyl styrene, and bromo-para-methyl-styrene; ethylene propylene diene monomer rubber; and combinations and copolymers thereof.
4. The process of claim 1 , wherein the unsaturated organic polymer is in the form of latex particles or a polymer resin.
5. The process of claim 1 , wherein the sulfur containing cross linking agent is a hexasulfide, tetrasulfide, or disulfide compound or a copolymer thereof.
6. The process of claim 1 , wherein the sulfur containing cross linking agent is selected from the group consisting of polysulfide alkyl silanes, mercapto aryl silanes, polysulfide aryl silanes, silated core polysulfides, silated cyclic core polysulfides, sulfur-containing silanes, sulfanylsilanes, sulfur-containing siloxanes, sulfur-functional polyorganosiloxanes, bis(triethoxysilylpropyl) tetrasulfide (TESPT), 3-thiocyanatopropyltriethoxysilane, 3-mercaptopropyltrimethoxysilane and any combination thereof.
7. The process of claim 1 , wherein the sulfur containing cross linking agent is a sulfidosilane of a general formula (R 1 —O) 3 —Si—R 2 —S x —R 2 —Si—(R 1 —O) 3 or of a general formula HS—R 1 —Si—(O—R 2 ) 3 where R 1 and R 2 are same or different alkyl or aryl groups; and wherein x is a number between 1 and 8.
8. The process of claim 1 wherein the organic polymer bound to the silica network comprises up to 50 wt % of the gel composition.
9. The process of claim 1 wherein the sulfur containing crosslinker comprises up to 50 wt % of the gel composition.
10. The process of claim 1 wherein the organic polymer bound to the silica network comprises at least 3 wt % of the gel composition.
11. The process of claim 2 wherein the drying is performed using a supercritical fluid.
12. The process of claim 1 further comprising a step of drying the gel composition to produce an aerogel composition.
13. The process of claim 1 further comprising a step of incorporating fibers into the gel composition.
14. The process of claim 1 further comprising a step of incorporating fibers into the gel composition; and a step of drying the gel composition to produce an aerogel composition.