Microporous polyolefin-based aerogels

Patent metadata

Field	Value
Publication number	US-2016272777-A1
Application number	US-201414549946-A
Country	US
Kind code	A1
Filing date	Nov 21, 2014
Priority date	Apr 7, 2005
Publication date	Sep 22, 2016
Grant date	—

Abstract

Microporous polyolefin and microporous polydicyclopentadiene (polyDCPD) based aerogels and methods for preparing and using the same are provided. The aerogels are produced by forming a polymer gel structure within a solvent from a olefin or dicyclopentadiene monomer via Ring Opening Metathesis Polymerization (ROMP) reactions, followed by supercritical drying to remove the solvent from the aerogel. Other aerogels are prepared by sequentially (1) mixing at least one dicyclopentadiene monomer, at least one solvent at least one catalyst and at least one inorganic and/or organic reinforcing material, (2) gelling the mixture, (3) aging, and (4) supercritical drying. Aerogels provided herein are inexpensive to prepare, possess desirable thermal, mechanical, acoustic, chemical, and physical properties and are hydrophobic. The aerogels provided herein are suitable for use in various applications, including but not limited to thermal and acoustic insulation, radiation shielding, and vibrational damping applications.

First claim

1 . A porous polydicyclopentadiene based aerogel material comprising a polydicyclopentadiene polymer; wherein the porous polydicyclopentadiene based aerogel material has a density from 0.01 g/cm 3 to about 0.6 g/cm 3 .

2 . The material of claim 1 , wherein the polydicyclopentadiene polymer comprises at least one polydicyclopentadiene monomeric unit represented by Formula I:

wherein R1 and R2 comprise one or more additional polydicyclopentadiene monomeric units; and wherein m is a positive integer.

3 . The material of claim 1 , wherein the polydicyclopentadiene polymer comprises at least one polydicyclopentadiene monomeric unit represented by Formula II:

wherein R3, R4, R5 and R6 comprise one or more additional polydicyclopentadiene monomeric units; and wherein n is a positive integer.

4 . The material of claim 1 , wherein the polydicyclopentadiene polymer comprises at least one polydicyclopentadiene monomeric unit represented by Formula I:

wherein R1 and R2 comprise one or more additional polydicyclopentadiene monomeric units, and wherein m is a positive integer; and at least one polydicyclopentadiene monomeric unit represented by Formula II:

wherein R3, R4, R5 and R6 comprise one or more additional polydicyclopentadiene monomeric units, and wherein n is a positive integer.

5 . The material of claim 3 , wherein the porous polydicyclopentadiene based aerogel material is composed of cross-linked polydicyclopentadiene polymers, and between 0.0001% and 5% by weight of a transition metal selected from niobium, tantalum, chromium, molybdenum, tungsten, rhenium, iron, ruthenium, osmium, or a mixture thereof.

6 . The material of claim 5 , wherein the transition metal is between 0.001% and about 1% by weight of the porous material and the transition metal is selected from molybdenum, tungsten, rhenium, ruthenium, or osmium, or a mixture thereof.

7 . The material of claim 1 , wherein the porous polydicyclopentadiene based aerogel material comprises cross-linked polydicyclopentadiene polymers and at least one reinforcement material selected from the group consisting of fibers, fiber aggregates, nonwoven fabrics, woven fabrics, fibrous batting, lofty fibrous batting, nonwoven fibrous batting, particles and combinations thereof.

8 . The material of claim 7 , further comprising at least one additive selected from the group consisting of IR opacifiers, antioxidants, flame retardant agents, organic or inorganic fillers, crosslinking agents, elastomers, binders, plasticizers, pigments, dyes and combination thereof.

9 . The material of claim 1 , wherein the porous aerogel material is prepared by the steps comprising: (a) mixing at least one olefin feedstock comprising at least one dicyclopentadiene monomer, a polymerization catalyst, and at least one solvent to form a mixture; (b) maintaining the mixture in a quiescent state at a temperature suitable for gel formation until the mixture forms a gel; and (c) drying the gel, thereby obtaining the porous polydicyclopentadiene based aerogel material.

10 . An article comprising the porous polydicyclopentadiene based aerogel material of claim 1 and a vacuum-sealed envelope, package or container; wherein the porous polydicyclopentadiene based aerogel material is incorporated into the vacuum-sealed envelope, package or container.

11 . A porous polynorbornadiene based aerogel material comprising a polynorbornadiene polymer; wherein the porous polynorbornadiene based aerogel material has a density from 0.01 g/cm 3 to about 0.6 g/cm 3 .

12 . The material of claim 11 , wherein the polynorbornadiene polymer comprises at least one polynorbornadiene monomeric unit represented by Formula III:

wherein R7 and R8 comprise one or more additional polynorbornadiene monomeric units; and wherein p is a positive integer.

13 . The material of claim 11 , wherein the polynorbornadiene polymer comprises at least one polynorbornadiene monomeric unit represented by Formula IV:

wherein R9, R10, R11 and R12 comprise one or more additional polynorbornadiene monomeric units; and wherein r is a positive integer.

14 . The material of claim 11 , wherein the polynorbornadiene polymer comprises at least one polynorbornadiene monomeric unit represented by Formula III:

wherein R7 and R8 comprise one or more additional polynorbornadiene monomeric units, and wherein p is a positive integer; and at least one polynorbornadiene monomeric unit represented by Formula IV:

wherein R9, R10, R11 and R12 comprise one or more additional polynorbornadiene monomeric units, and wherein r is a positive integer.

15 . The material of claim 13 , wherein the porous polynorbornadiene based aerogel material is composed of cross-linked polynorbornadiene polymers, and between 0.0001% and 5% by weight of a transition metal selected from niobium, tantalum, chromium, molybdenum, tungsten, rhenium, iron, ruthenium, osmium, or a mixture thereof.

16 . The material of claim 15 , wherein the transition metal is between 0.001% and about 1% by weight of the porous material and the transition metal is selected from molybdenum, tungsten, rhenium, ruthenium, or osmium.

17 . The material of claim 11 , wherein the porous polynorbornadiene based aerogel material is composed of the cross-linked polynorbornadiene polymers and at least one reinforcement material selected from the group consisting of fibers, fiber aggregates, nonwoven fabrics, woven fabrics, fibrous batting, lofty fibrous batting, nonwoven fibrous batting, particles and combinations thereof.

18 . The material of claim 17 , further comprising at least one additive selected from the group consisting of IR opacifiers, antioxidants, flame retardant agents, organic or inorganic fillers, crosslinking agents, elastomers, binders, plasticizers, pigments, dyes and combination thereof.

19 . The material of claim 11 , wherein the porous aerogel material is prepared by the steps comprising: (a) mixing at least one olefin feedstock comprising at least one norbornadiene monomer, a polymerization catalyst, and at least one solvent to form a mixture; (b) maintaining the mixture in a quiescent state at a temperature suitable for gel formation until the mixture forms a gel; and (c) drying the gel, thereby obtaining the porous polynorbornadiene based aerogel material.

20 . An article comprising the microporous polynorbornadiene based material of claim 11 and a vacuum-sealed envelope, package or container; wherein the porous polynorbornadiene based material is incorporated into the vacuum-sealed envelope, package or container.

21 . (canceled)

22 . (canceled)

Assignees

• Aspen Aerogels Inc

Inventors

• Lee Je Kyun
• Gould George L

Classifications

• C08F34/00 Primary

  Homopolymers and copolymers of cyclic compounds having no unsaturated aliphatic radicals in a side chain and having one or more carbon-to-carbon double bonds in a heterocyclic ring (cyclic esters of polyfunctional acids C08F18/00; cyclic anhydrides or imides C08F22/00) · CPC title

• C08G2261/3325

  derived from other polycyclic systems · CPC title

• C08J2203/08

  Supercritical fluid · CPC title

• C08J2355/00

  Characterised by the use of homopolymers or copolymers, obtained by polymerisation reactions only involving carbon-to-carbon unsaturated bonds, not provided for in groups C08J2323/00 - C08J2353/00 · CPC title

• C08J9/28 Primary

  by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum · CPC title