POLYPHOSPHATE MATERIALS
20240391775 ยท 2024-11-28
Inventors
- JUNJI SAKAMOTO (Cambridge, MA, US)
- Alexei TEN (Cambridge, MA, US)
- Mohamad KODAIMATI (Cambridge, MA, US)
- Haihui Joy JIANG (Cambridge, MA, US)
- Amit Arun NAGARKAR (Boston, MA, US)
- Samuel E. ROOT (Cambridge, MA, US)
- George M. WHITESIDES (Cambridge, MA, US)
Cpc classification
International classification
Abstract
A polyphosphate material is disclosed. The polyphosphate material can include a plurality of polyphosphate chains. The polyphosphate chains can have a backbone that include oxygen-phosphate bonds. Two or more cations can be included. Further, the polyphosphate material can be amorphous. The two or more cations can be monovalent cations, divalent cations, trivalent cations, tetravalent cations, and combinations thereof. The two or more cations can be lithium, sodium, potassium, rubidium, cesium, francium, ammonium, beryllium, magnesium, calcium, strontium, barium, radium, zinc, titanium, iron (Fe.sup.2+), chromium (Cr.sup.2+), manganese (Mn.sup.2+), cobalt (Co.sup.2+), nickel (Ni.sup.2+), copper (Cu.sup.2+), cadmium, tin (Sn.sup.2+), mercury (Hg.sup.2+), lead (Pb.sup.2+), aluminum, boron, gallium, iron (Fe.sup.+3), chromium (Cr.sup.+3), cobalt (Co.sup.+3), gold (Au.sup.+3), antimony (Sb.sup.+3), nickel (Ni.sup.+3), bismuth (Bi.sup.+3), manganese (Mn.sup.+3) zirconium, silicon, and combinations of thereof. The two or more cations can be monovalent cations. The two or more cations can be sodium and potassium or potassium and lithium.
Claims
1. A polyphosphate material comprising: a plurality of polyphosphate chains having a backbone comprising oxygenphosphate bonds; and two or more cations, wherein the polyphosphate material is amorphous.
2. The polyphosphate material of claim 1, wherein the two or more cations are selected from a group consisting of monovalent cations, divalent cations, trivalent cations, tetravalent cations, and combinations thereof.
3. The polyphosphate material of claim 1, wherein the two or more cations are selected from the group consisting of lithium, sodium, potassium, rubidium, cesium, francium, ammonium, beryllium, magnesium, calcium, strontium, barium, radium, zinc, titanium, iron (Fe.sup.2+), chromium (Cr.sup.2+), manganese (Mn.sup.2+), cobalt (Co.sup.2+), nickel (Ni.sup.2+), copper (Cu.sup.2+), cadmium, tin (Sn.sup.2+), mercury (Hg.sup.2+), lead (Pb.sup.2+), aluminum, boron, gallium, iron (Fe.sup.3+), chromium (Cr.sup.3+), cobalt (Co.sup.3+), gold (Au.sup.3+), antimony (Sb.sup.3+), nickel (Ni.sup.3+), bismuth (Bi.sup.3+), manganese (Mn.sup.3+), zirconium, silicon, manganese (Mn.sup.4+), titanium (Ti.sup.4+), and combinations of thereof.
4. The polyphosphate material of claim 1, wherein the two or more cations comprise monovalent cations.
5. The polyphosphate material of claim 1, where the two or more cations comprise sodium and potassium.
6. The polyphosphate material of claim 1, wherein the two or more cations comprise potassium and lithium.
7. The polyphosphate material of claim 1, wherein the polyphosphate material has a glass transition temperature of less than 250 C.
8. The polyphosphate material of claim 1, wherein the polyphosphate material has a melting temperature less than 500 C.
9. The polyphosphate material of claim 1, wherein the polyphosphate material is transparent.
10. The polyphosphate material of claim 1, wherein the polyphosphate material is a gel.
11. The polyphosphate material of claim 10, wherein the gel comprises charged particles.
12. The polyphosphate material of claim 1, wherein the polyphosphate material is a thermoplastic material.
13. The polyphosphate material of claim 1, wherein the polyphosphate material is an adhesive.
14. The polyphosphate material of claim 1, wherein the polyphosphate material is a film.
15. The polyphosphate material of claim 1, wherein the polyphosphate material is hydrophobic.
16. The polyphosphate material of claim 1, further comprising hydrophobic cations.
17. The polyphosphate material of claim 1, further comprising a dissolved metal salt.
18. The polyphosphate material of claim 17, wherein the dissolved metal salt is selected from the group comprising copper salts, magnesium salts, chromium salts, europium salts, iron salts, titanium salts, chromium salts, manganese salts, cobalt salts, nickel salts, tin salts, mercury salts, lead salts, chromium salts, cobalt salts, gold salts, antimony salts, bismuth salts, and combinations thereof.
19. A method of forming a polyphosphate material comprising: adding a polyphosphate powder comprising a first cation to a solution of a salt of a second cation; heating the solution to dissolve the polyphosphate powder; cooling the solution to cause phase separation into an upper liquid layer and a lower liquid layer, wherein the lower liquid layer comprises a coacervate of polyphosphate; and collecting the coacervate.
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29. A method of forming a polyphosphate material comprising: providing a first phosphate monomer comprising a first cation; providing a second phosphate monomer comprising a second cation; heating the first phosphate monomer and second phosphate monomer to form a liquid; and cooling the liquid to form an amorphous polyphosphate material.
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44. A polyphosphate material comprising: a plurality of polyphosphate chains having a backbone comprising oxygenphosphate bonds; and one or more multivalent cations forming crosslinks between the polyphosphate chains, wherein the polyphosphate material is porous.
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64. A method of forming a polyphosphate material comprising: providing a mixture of a phosphate monomer comprising a multivalent cation; and heating the mixture to form a polyphosphate foam.
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Description
BRIEF DESCRIPTION OF THE DRAWINGS
[0016] The objects and advantages will be apparent upon consideration of the following detailed description, taken in conjunction with the accompanying drawings, in which like reference characters refer to like parts throughout, and in which:
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DETAILED DESCRIPTION
[0118] Disclosed herein are polyphosphate materials with practical application to bulk materials. The thermal stability and the polyelectrolytic/chelating characters of polyphosphate materials can combine heat resistance and fire resistance of these materials with interesting optical, thermal, and mechanical properties. Disclosed herein are polyphosphate materials with properties based on multivalent interactions of polyphosphate chains with metal ions, charged nanoparticles, or surfaces of other bulk materials. Disclosed herein are methods of making polyphosphate processable into a range of bulk materials including anti-fire coatings, soft materials, adhesives, luminescent solid solutions, and thermally insulating porous materials. For example, by selecting metal cations or combinations of metal cations used in forming polyphosphate materials and methods forming polyphosphate materials, polyphosphate materials can be formed as amorphous materials, plasticized materials, gels, adhesives, films, or foams.
[0119] Disclosed herein is a thermal polycondensation of orthophosphate for the synthesis of polycondensation. Potential advantages of utilizing the synthesis disclosed herein include: (i) being free from any reagents and solvents; (ii) the starting material can be inexpensive and non-toxic; (iii) the product polymer can hydrolyze back to the starting material; (iv) the polymerization process generates only water as a side product, and the back reaction (i.e. hydrolysis) requires only water. Disclosed herein are methods to tune properties of polyphosphate with a selection of counter ions (e.g., cations) and to process polyphosphate by both wet and dry processes into desired shapes and morphologies.
[0120] Polyphosphate materials disclosed herein are polyelectrolytes with a thermally stable molecular structure, which, in some embodiments, combine heat and fire resistance of polyphosphate materials with interesting optical, thermal, and mechanical properties. As disclosed herein, these properties can be modified using multivalent interactions of polyphosphate chains with metal ions, charged nanoparticles, or surfaces of other bulk materials. For example, a porous monolithic material that includes polyphosphate chains held together with Al.sup.3+ can have both thermal insulation properties and stability over a wide temperature range from 196 to 800 C. Polyphosphates can be non-flammable, less expensive, more environmentally friendly, and easier to produce and recycle, compared to existing thermal insulating materials. For example, porous material of polyphosphate can be useful for a range of insulation purposes that include the protection of vehicles in aerospace industries and the reduction of thermal energy loss in power industries. In some embodiments, polyphosphate materials disclosed herein can be more processible or can used as adhesives. For example, plasticized polyphosphates can be more processible or can used as adhesives
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[0123] In some embodiments, the polyphosphate materials disclosed herein can withstand high temperatures. In some embodiments, polyphosphate materials are polyphosphate foams that can withstand temperatures of up to 700 C., up to 800 C., or up to 900 C. over at least several hours. In some embodiments, polyphosphate materials are polyphosphate foams that decompose at temperatures of at least 900 C. or at least 1000 C. over a prolonged period of time (e.g., days). In some embodiments, polyphosphate materials can be nonflammable and less prone to react with oxygen in air. In some embodiments, polyphosphates can be used as flame retardants, optionally with additional additives. As shown in
[0124] In some embodiments, the polyphosphate materials disclosed herein can also withstand extremely low temperatures. In some embodiments, polyphosphate materials can withstand temperatures corresponding to that of liquid nitrogen. In some embodiments, polyphosphate foams can withstand temperatures of less than 0 C., 50 C., 60 C., 70 C., or 80 C., 100 C., 150 C., 180 C. or a temperature in any range bounded by any value disclosed herein. In some embodiments, polyphosphate materials can withstand temperatures of less than 0 C., 78 C. or 196 C.
[0125] In some embodiments, the polyphosphate materials disclosed herein can be biodegradable or have biodegradability properties. For example, enzymes such as exopolyphosphatase (EC 3.6.1.11) catalyze the hydrolysis of polyphosphate into orthophosphate. In some embodiments, as shown in
I. Synthesis of Polyphosphate Materials
[0126] In some embodiments, polyphosphates can be formed using a simple dehydration or condensation reaction, as shown in
[0127] In some embodiments, polyphosphate materials can be synthesized using phosphate monomers and cations. In some embodiments, the cation is monovalent, e.g., a monovalent metal. In some embodiments, the cation is divalent, e.g., a divalent metal. In some embodiments, the cation is trivalent, e.g., a trivalent metal such as Fe.sup.3+. In some embodiments, the cation is tetravalent, e.g., a tetravalent metal such as manganese (Mn.sup.4+), titanium (Ti.sup.4+), and/or Sn.sup.4+. In some embodiments, by selecting the metal cation or combination of metal cations, the properties of the polyphosphate materials can be altered to make these materials more processible or to have desired properties.
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[0131] In some embodiments, shown in
[0132] In other embodiments, shown in
[0133] In some embodiments, phosphate materials can be formed by coacervation. Coacervation results in phase separation, as shown in
[0134] In some embodiments, polyphosphate-based coacervates can be used in applications including wastewater treatment, protein purification, food formulation, drug delivery, and cellular mimics. In some embodiments, the polyphosphate-based coacervates can include mixed cations. In some embodiments, the polyphosphate-based coacervates are liquid. It can turn to be a plastic material when isolated and dried.
II. Polyphosphate Materials
[0135] In some embodiments, a polyphosphate material includes an oxygen-phosphate backbone. In some embodiments a polyphosphate material includes molecular groups in addition to oxygen and phosphate in the backbone. In some embodiments, a polyphosphate material includes orthophosphate residues as repeating units. In some embodiments, polyphosphate materials include a polyphosphate polymer chain having a backbone of oxygen-phosphate bonds. In some embodiments, a polyphosphate material includes one or more counterions (e.g., cations). In some embodiments, a polyphosphate material's precursors include phosphate monomers. Exemplary phosphate monomers include dihydrogen phosphate salts.
[0136] In some embodiments, a polyphosphate material includes one or more cations as counterions. In some embodiments, the cations include monovalent cations. Exemplary monovalent cations include Group I cations and/or those outside of Group I such as gold (Au.sup.+), silver, and/or copper (Cu.sup.+). Exemplary monovalent cations include lithium, sodium, potassium, rubidium, cesium, francium, ammonium, and combinations thereof. In some embodiments, the cations include divalent cations. Exemplary divalent cations include group II cations. Exemplary divalent cations include beryllium, magnesium, calcium, strontium, barium, radium, zinc, titanium, iron (Fe.sup.2+), chromium (Cr.sup.2+), manganese (Mn.sup.2+), cobalt (Co.sup.2+), nickel (Ni.sup.2+), copper (Cu.sup.2+), cadmium, tin (Sn.sup.2+), mercury (Hg.sup.2+), lead (Pb.sup.2+), and combinations thereof. In some embodiments, the cations include trivalent cations. Exemplary trivalent cations include group XIII cations. Exemplary trivalent cations include aluminum, boron, gallium, iron (Fe.sup.3+), chromium (Cr.sup.3+), cobalt (Co.sup.3+), gold (Au.sup.3+), antimony (Sb.sup.3+), nickel (Ni.sup.3+), bismuth (Bi.sup.3+), manganese (Mn.sup.3+), and combinations thereof. In some embodiments, the cations include tetravalent cations. Exemplary tetravalent cations include zirconium, silicon, manganese (Mn.sup.4+), titanium (Ti.sup.4+), and combinations thereof. In some embodiments, a polyphosphate includes two or more different cations, for example, two, three, or four cations, or any number of cations in a range bounded by any value disclosed herein. In some embodiments, a polyphosphate includes a combination of monovalent, divalent, trivalent, and tetravalent cations. In some embodiments, the one or more cations include iron. In some embodiment, inclusion of iron ions contributes to magnetic properties of the polyphosphate material. In some embodiments, iron is a counterion of the phosphate material. In other embodiments, iron is added in smaller amounts and dissolved in a melt of polyphosphate.
[0137] In some embodiments, a melt of polyphosphate material can dissolve a variety of metal salts. Non-limiting examples of metal salts include salts of multivalent cations, e.g., divalent, trivalent, or tetravalent cations. Non-limiting examples of metal salts include salts of copper, magnesium, chromium, europium, titanium, iron, chromium, manganese, cobalt, nickel, cadmium, tin, mercury, lead, chromium, cobalt, gold, antimony, bismuth, and combinations thereof. Non-limiting examples of metal salts include CuCl.sub.2, MnSO.sub.4, and CrCl.sub.3, EuCl.sub.3, and combinations thereof. In some embodiments, inclusion of metal salts can alter the color of the polyphosphate material. For example, metal cations can contribute color by forming coordination complexes. In some embodiments, inclusion of metal cations, such as fluorescent metal complexes, results in fluorescence of the polyphosphate material. Non-limiting examples of metal salts that result in fluorescence include EuCl.sub.3. Non-limiting examples of metal salts that can result in fluorescence include lanthanoids, e.g., lanthanum (e.g., Ln.sup.3+), terbium (Tb.sup.3+), and gadolinium (Gd.sup.3+).
A. Plasticized Polyphosphates
[0138] In one aspect, a polyphosphate material includes a plurality of polyphosphate chains having a backbone comprising oxygen-phosphate bonds; and two or more cations, wherein the polyphosphate material is amorphous.
[0139] In some embodiments, plasticized polyphosphate materials can be formed by incorporating two or more cations to a polyphosphate material. For example, incorporating two or more different cations can inhibit crystallization so that the resultant material becomes more moldable and melt processible. In some embodiments, a plasticized phosphate material is characterized X-ray diffraction (XRD), dynamic mechanical analysis (DMA), differential scanning calorimetry (DSC). For example, a plasticized polyphosphate material can be identified by the absence of distinct peaks in an XRD spectra. As another example, a discontinuous change of properties of the plasticized polyphosphate is observed by using DSC and/or DMA due to glass transition or melting. In these embodiments, incorporating two or more different cations can inhibit crystallization of long polymer chains of the polyphosphate material, resulting in an amorphous material. In some embodiments, incorporating two different cations of different sizes can disrupt order and inhibit crystallization. In contrast, when a polyphosphate material is formed using a single cation (e.g., a homo-polyphosphate), the polyphosphate is typically crystalline or semi-crystalline, hard, brittle, and opaque.
[0140] In some embodiments, incorporating a two or more cations can result in the melting point temperature of the mixed-polyphosphate being lower than the melting temperatures of homo-polyphosphates. For example, incorporating the two or more cations can decrease the melting temperature of a polyphosphate material. As a result, such polyphosphate materials can be more processible in a melt at a lower temperature, making them easier to shape into a desired shape. For example, plasticized polyphosphate materials can have a melting temperature less than 300 C. In some embodiments, plasticized polyphosphate materials can have a melting temperature of about 180 C., 190 C., 200 C., 210 C., 220 C., 230 C., 240 C., 250 C., 260 C., 270 C., 280 C., 290 C., 300 C. or any temperature in a range bounded by any value disclosed herein. In some embodiments, plasticized polyphosphate materials can have a melting temperature of about 200 to about 250 C. In comparison, potassium polyphosphate has a melting temperature greater than 1000 C.
[0141] In some embodiments, incorporating a two or more cations can result in a lower glass transition temperature of a polyphosphate material. Polyphosphate materials with lower glass transition temperatures can be processed at lower temperatures compared to those with a high transition temperature. In some embodiments, plasticized polyphosphate materials can have a glass transition temperature of about 180 C., 190 C., 200 C., 210 C., 220 C., 230 C., 240 C., 250 C., 260 C., 270 C., 280 C., 290 C., 300 C. or any value in a range bounded by any value disclosed herein. In some embodiments, plasticized polyphosphate materials can have a glass transition temperature of about 200 to about 250 C. In some embodiments, plasticized polyphosphate materials have a glass transition temperature (T.sub.g) of about 220 C. In some embodiments, the glass transition temperature depends on the combination of cations or the ratio of cations.
[0142] In some embodiments, a plasticized polyphosphate material is non-flammable. For example, plasticized polyphosphates generally do not burn when exposed to flame. For example, a plasticized polyphosphate material is more thermally stable than a carbon-based polymer.
[0143] In some embodiments, a plasticized phosphate material can be transparent. In some embodiments, the transparency of a plasticized phosphate material can be controlled by the rate at which the material is cooled from a melt. Above the melting temperature, a polyphosphate material incorporating two or more cations is transparent. In some embodiments, quickly cooling this phosphate material can result in an amorphous, transparent material, for example, because the polyphosphate chains do not have time to crystallize or become ordered and therefore remain amorphous. In some embodiments, cooling a polyphosphate material over a time period on the order of minutes to less than an hour can result in an amorphous, transparent polyphosphate material. In some embodiments, cooling more slowly can result in a translucent or opaque material, for example, if the polyphosphate chains are allowed sufficient time to crystallize or become ordered, rather than forming an amorphous polyphosphate. In some embodiments, the transparency can be controlled by the choice of cations, for example, by choosing a combination of cations that decreases crystallinity or increases disorder of the polyphosphate chains. In some embodiments, transparency depends on the combination of cations or the ratio of cations. For example, a potassium lithium polyphosphate will be transparent even if cooled slowly.
[0144] In some embodiments, a plasticized polyphosphate material includes two or more monovalent cations. In some embodiments, a plasticized polyphosphate material includes two or more monovalent cations with different sizes. For example, a plasticized phosphate can include two or more of lithium, sodium, potassium, rubidium, cesium, francium, and ammonium. Non-limiting examples of a plasticized polyphosphate material with monovalent cations include potassium lithium phosphate and potassium lithium phosphate. In some embodiments, a plasticized polyphosphate includes three monovalent cations, e.g., sodium, lithium, and potassium. In some embodiments, at the same ratio, a potassium lithium phosphate will have a greater decrease in crystallinity compared to a potassium sodium phosphate.
[0145] In some embodiments, a plasticized polyphosphate material can include multivalent cations. In some embodiments, a plasticized polyphosphate material can include two or more divalent cations. Exemplary divalent cations include group II cations. Exemplary divalent cations include beryllium, magnesium, calcium, strontium, barium, radium, zinc, titanium, iron (Fe.sup.2+), chromium (Cr.sup.2+), manganese (Mn.sup.2+), cobalt (Co.sup.2+), nickel (Ni.sup.2+), copper (Cu.sup.2+), cadmium, tin (Sn.sup.2+), mercury (Hg.sup.2+), lead (Pb.sup.2+), and combinations thereof. In some embodiments, a plasticized polyphosphate material can include two or more trivalent cations. Exemplary trivalent cations include group XIII cations. Exemplary trivalent cations include aluminum, boron, gallium, iron (Fe.sup.3+), chromium (Cr.sup.3+), cobalt (Co.sup.3+), gold (Au.sup.3+), antimony (Sb.sup.3+), nickel (Ni.sup.3+), bismuth (Bi.sup.3+), manganese (Mn.sup.3+), and combinations thereof. In some embodiments, a plasticized polyphosphate a combination of cations of different valences, for example, at least two of monovalent cations, divalent cations, or trivalent cations.
[0146] In some embodiments, the cations have a ratio of 1:1 mol/mol. In some embodiments, the cations have a ratio of 1:2 mol/mol. In some embodiments, the cations have a ratio of 3:1 mol/mol. For example, in preparing lithium potassium polyphosphate at 500 C., material with a mixing ration (Li/K) in the range of 1:2 mol/mol to 3:1 mol/mol can be amorphous where a cooling rate of the polyphosphate may be taken into account.
[0147] In one aspect, a method of forming a polyphosphate material includes adding a polyphosphate powder comprising a first cation to a solution of a salt of a second cation; heating the solution to dissolve the polyphosphate powder; cooling the solution to cause phase separation into an upper liquid layer and a lower liquid layer, wherein the lower liquid layer comprises a coacervate of polyphosphate; and collecting the coacervate.
[0148] In some embodiments, plasticized phosphates can be formed by coacervation. Coacervates can form when a polyphosphate powder of a first metal cation is added to a solution of a solution of salt of a second metal cation and heated or boiled to dissolve the polyphosphate powder. The polyphosphate powder can be heated to a temperature of less than or above 100 C. The second cation can then exchange with a portion of the first cation to form a mixed-phosphate with both the first cation and the second cation. The first cation can be potassium and the second cation can be sodium or lithium. Though, this is for example purposes only and should not be construed as a limitation. When the solution is cooled, the solution will phase separate into two layers, and the lower layer is a coacervate of polyphosphate. For example, a potassium polyphosphate can be added to a solution of sodium chloride to form a potassium sodium phosphate. In some embodiments, the coacervate can be dried to form a waxy, plasticized material. In some embodiments, the dried coacervate can be ground into a powder.
[0149] In one aspect, a method of forming a polyphosphate material includes providing a first phosphate monomer comprising a first cation; providing a second phosphate monomer comprising a second cation; heating the first phosphate monomer and second phosphate monomer to form a liquid; and cooling the liquid to form an amorphous polyphosphate material. The amorphous polyphosphate material can be dissolved into water. Further, the solution can be gelled by adding a crosslinking material.
[0150] In some embodiments, plasticized phosphates can be formed by heating a mixture of a first monomer having a first metal cation (e.g., a metal dihydrogen phosphate) and a second monomer having a second metal cation (e.g., a metal dihydrogen phosphate) to form a liquid (e.g., a melt). Non-limiting examples of monomers include LiH.sub.2PO.sub.4, NaH.sub.2PO.sub.4, and KH.sub.2PO.sub.4. In some embodiments, the mixture is heated at a temperature between 350 C. and 1000 C. In some embodiments, heating at a higher temperature results in a shorter reaction time. In some embodiments, the mixture is heated at a temperature of about 350 C., 400 C., 450 C., 500 C., 550 C., 600 C., 650 C., 700 C., 750 C., 800 C., 850 C., 900 C., 950 C., 1000 C., or any value in a range bounded by a value disclosed herein. In some embodiments, the mixture is heated at a temperature of 1000 C. In some embodiments, the mixture is heated in an oven or by a flame. This liquid can be cooled to form a solid polyphosphate material. In some embodiments, a this solid can be ground to a powder.
[0151] In some embodiments, a polyphosphate powder with two or more cations can be mixed with metal salt and heated to a transparent liquid to dissolve additional metal salts. Non-limiting examples of metal salts include salts of copper, magnesium, chromium, europium, iron, titanium, chromium, manganese, cobalt, nickel, tin, mercury, lead, chromium, cobalt, gold, antimony, bismuth, and combinations thereof. Non-limiting examples of metal salts include CuCl.sub.2, MnSO.sub.4, and CrCl.sub.3, EuCl.sub.3, Fe.sub.2(SO.sub.4).sub.3, and combinations thereof. In some embodiments, inclusion of metal salts can alter the color of the polyphosphate material. For example, metal cations can contribute color by forming coordination complexes. In some embodiments, inclusion of metal cations results in fluorescence of the polyphosphate material. Non-limiting examples of metal salts that result in fluorescence include EuCl.sub.3. Non-limiting examples of metal salts that can result in fluorescence include lanthanoids, e.g., lanthanum (e.g., Ln.sup.3+), terbium (Tb.sup.3+), and gadolinium (Gd.sup.3+).
[0152] In some embodiments, a plasticized polyphosphate material is a polyphosphate gel. In some embodiments, addition of multivalent cations or charged particles to an aqueous solution of a polyphosphate can cause formation of a polyphosphate hydrogel. In some embodiments, a polyphosphate gel can be formed by placing a polyphosphate material of a first cation into a solution of a salt of a second cation. For example, a polyphosphate powder of a first metal cation can be added to a solution of a solution of salt of a second metal cation and boiled to dissolve the polyphosphate powder. The cations can exchange such that the polyphosphate material is a mixed-polyphosphate including both the first cation and the second cation, and the solution of the polyphosphate can gel when mixed with crosslinking material. In some embodiments, the polyphosphate gel can be crosslinked using charged particles, for example, by mixing the polyphosphate coacervate with a dispersion of charged particles in water and mixing to form a gel, with the metal charged particles acting as crosslinks. In some embodiments, a gel can be formed by adding charged particles to an aqueous solution of polyphosphate, with charged particles acting as crosslinks. In some embodiments, charged particles form crosslinks via electrostatic interaction with the polyphosphate material. For example, a positively charged particle can interact with the negatively charged polyphosphate backbone. Non-limiting examples of charged polyelectrolytes include metal oxide nanoparticles, dendrimers (e.g., dendrimers with ammonium groups), and chitosan. Non-limiting examples of metal oxide nanoparticles include zinc oxide, titania, and combinations thereof.
[0153] In some embodiments, plasticized polyphosphate materials can be used as an adhesive. In some embodiments, a polyphosphate coacervate or polyphosphate solution can be used as an adhesive. In these embodiments, the coacervate or polyphosphate solution can be heated to remove excess water and form an adhesive. In some embodiments, when a plasticized polyphosphate is heated, it forms a viscous fluid. This fluid can be applied to two substrates to adhere them together. Once cooled, the plasticized polyphosphate material forms a glue or adhesive. In some embodiments, this adhesive is thermoplastic, rather than thermoset, and can come apart when heated again, for example at a temperature above the melting temperature, or dipped in water. In some embodiments, a plasticized polyphosphate can be used as an adhesive for glass, metal, ceramic, paper, or wood materials. In some embodiments, a plasticized polyphosphate can be used as an adhesive for a material that is capable of forming coordination, electrostatic and/or hydrogen bonds. In some embodiments, a plasticized polyphosphate can be used as an adhesive between two different materials, for example glass and ceramic.
[0154] In some embodiments, plasticized polyphosphate materials can form films. In some embodiments, films can be formed by placing a plasticized polyphosphate material on a heat press and applying pressure at a temperature greater than T.sub.g. In some embodiments, these films can be transparent. In some embodiments, films can be formed by drying a concentrated solution of polyphosphate on a substrate, e.g., a Teflon substrate. In some embodiments, films can be formed by spin coating a substrate, e.g., by spin coating a silicon wafer.
[0155] In some embodiments, plasticized polyphosphate materials can be made hydrophobic by exchanging cations of the polyphosphate material with hydrophobic cations, e.g., tetraalkyl ammonium ions, in solution. For example, an aqueous solution of a polyphosphate with two cations (e.g., sodium-potassium polyphosphate) can be added to an aqueous solution of hydrophobic cations. In these embodiments, ion exchange can result in precipitation of a hydrophobic polyphosphate material. In some embodiments, hydrophobic plasticized polyphosphate materials can be made by exchanging alkali metal ions with substituted ammonium ions. In some embodiments, a hydrophobic cation is a cation that includes a hydrocarbon. Non-limiting examples of hydrophobic cations include mono-, di-, tri-, tetra-substituted ammonium cations and their perfluoro analogs. Non-limiting examples of hydrophobic cation include substituted ammonium (e.g., cetyltrimethylammonium, alkylammoniums), pyrrolium, imidazolium cations, and combinations thereof.
[0156] In some embodiments, a plasticized polyphosphate coating can be formed using a coacervate or a polyphosphate solution. For example, by forming a plasticized polyphosphate coating from a coacervate or polyphosphate solution, the coating can be applied at a lower temperature. This can allow coating of temperature sensitive materials, e.g., paper or wood. In some embodiments, a plasticized polyphosphate material can be applied by spray coating. In other embodiments, a plasticized polyphosphate coating can be applied using a melt, for example to apply a coating to glass, metal, or ceramic or other heat-stable materials. In some embodiments, incorporation of two or more cations in a plasticized polyphosphate material allows coating from a melt at lower temperatures.
[0157] In some embodiments, the plasticized polyphosphate materials disclosed herein can be used in various applications, for example, adhesives, fire-proof coatings, solid state Li-ion conductors, electronic coatings, polymer solvents, shielding materials from oxygen, and transparent films.
B. Polyphosphate Foams
[0158] In one aspect, a polyphosphate material includes a plurality of polyphosphate chains having a backbone comprising oxygen-phosphate bonds; and one or more multivalent cations forming crosslinks between the polyphosphate chains, wherein the polyphosphate material is porous.
[0159] In some embodiments, polyphosphate foams can be formed by incorporating one or more multivalent cations. Multivalent cations can form crosslinks between phosphate chains because they can interact with more than one phosphate unit. When polyphosphate precursors are heated, water molecules formed by the condensation reaction evaporate, forming bubbles or voids, and these voids can be stabilized by crosslinks formed by the multivalent cations to form pores.
[0160] In some embodiments, polyphosphate foams include a porous structure dominated by macropores. In some embodiments, polyphosphate foams include pores with diameters on the order of about a few micrometers. In some embodiments, polyphosphate foams include pores with diameters greater than 1p m. In some embodiments, polyphosphate foams include pores with diameter of 1 m, 2 m, 3, m, 4 m, 5 m, 10 m, 15 m, 20 m, 25 m, 30 m, 35 m, 40 m, 45 m, 50 m, 55 m, 60 m, 70 m, 80 m, 90 m, 100 m, or any value in a range bounded by any value disclosed herein. In some embodiments, the pores can form a three-dimensional, interconnected network. For example, fluids can permeate through the interconnected network formed by the pores. In some embodiments aqueous solutions can permeate through the interconnected network. In some embodiments, organic solvents can permeate through the interconnected network. In some embodiments, a polyphosphate material can store such fluids in the pores.
[0161] In some embodiments, the polyphosphate material is a polyphosphate foam. In some embodiments, the polyphosphate foam can have low density. In some embodiments, polyphosphate foams have a density of less than 0.15 g/cm.sup.3. In some embodiments, the density is less than 0.10, less than 0.05, less than 0.01 g/cm.sup.3 or a density in any range bounded by any value disclosed herein. In some embodiments, the polyphosphate material can have high porosity. In some embodiments, the porosity is at least 70%, at least 80%, at least 90%, at least 95% or a porosity in any range bounded by any value disclosed herein. In some embodiments, the polyphosphate material can have a surface area of at least 0.5 m.sup.2/g.
[0162] In some embodiments, polyphosphate foams can be semi-crystalline. In some embodiments, incorporating a second cation to a polyphosphate foam can decrease crystallinity.
[0163] In some embodiments, polyphosphate foams include one or more multivalent cations. In some embodiments, polyphosphate foams include cations with a valency of at least three. In these embodiments, including a cation with a valency of at least three can allow formation of crosslinks that stabilize voids during synthesis. In some embodiments, the cations include trivalent cations. Exemplary trivalent cations include group XIII cations. Exemplary trivalent cations include aluminum, boron, gallium, iron (Fe.sup.3+), chromium (Cr.sup.3+), cobalt (Co.sup.3+), gold (Au.sup.3+), antimony (Sb.sup.3+), nickel (Ni.sup.3+), bismuth (Bi.sup.3+), manganese (Mn.sup.3+) and combinations thereof. In some embodiments, the cations include tetravalent cations. Exemplary tetravalent cations include zirconium, silicon, manganese (Mn.sup.4+), titanium (Ti.sup.4+), and combinations thereof.
[0164] In some embodiments, aluminum polyphosphate foams can be synthesized using monomers of aluminum dihydrogenphosphate and/or iron (III) dihydrogen phosphate.
[0165] In one aspect, a method of forming a polyphosphate material includes providing a mixture of a phosphate monomer comprising a multivalent cation; and heating the mixture to form a polyphosphate foam.
[0166] In some embodiments, phosphate precursors can be heated rapidly to form polyphosphate foam.
[0167] In some embodiments when polyphosphate materials are heated rapidly during synthesis, the resulting material can have low density, high porosity, or both. In some embodiments, porosity can be controlled using pressure, geometry, or both. For example, pressure of the air being blown onto the polymer surface can control macroscopic homogeneity of the material (e.g., to avoid large, mm-sized voids). For example, pressure of the air can cause large voids to collapse so that they do not remain in the material. In another example, geometry (e.g., the powder grind size) of the monomer used for polymerization influences the spatial homogeneity of the polycondensation process (e.g., how quickly and how easily can bubbles escape from the material). In some embodiments, the polyphosphate material is a polyphosphate foam.
[0168] In some embodiments, polyphosphate foams can be formed by a layer-by-layer process. In a layer-by-layer process, a powder of polyphosphate precursor with a multivalent cation (e.g., a monomer of phosphate with a multivalent cation) can be deposited on a surface and heated. In some embodiments the powder can be heated at a temperature between about 800 C. and about 2000 C. In some embodiments, polyphosphate foam forms by heating at a temperature of 800 C., 900 C., 1000 C., 1100 C., 1200 C., 1300 C., 1400 C., 1500 C., 1600 C., 1700 C., 1800 C., 1900 C., 2000 C., or at any temperature in a range bounded by any value disclosed herein. In some embodiments, a layer of powder can be deposited using a spray gun. In some embodiments, a layer of powder can be deposited using a shaker. In some embodiments, a filter is used to deposit powder based on particle size. In some embodiments, a layer of powder can be heated using a gas torch, e.g., using a MAPP torch with a flame temperature of about 2000 C. In some embodiments, a layer of powder can be heated in an oven, e.g., at temperatures of at least about 800 C. This process of depositing and heating can be repeated to form a monolithic block of polyphosphate foam layer by layer. In some embodiments, a layer can be 0.3-0.5 mm. In some embodiments, the resulting monolith can be cut into a desired shape, e.g., using a razor or a laser cutter. In some embodiments, forming a polyphosphate foam layer by layer can prevent formation of large voids remaining inside the material and thereby improve mechanical stability of the monolith. In some embodiments, a layer-by-layer process prevents formation of large voids because voids are limited by the thickness of the layers. For example, in a layer-by-layer process, the voids can have a size much less than the thickness of the layer. In some embodiments, a layer-by-layer process prevents large defects, e.g., large voids, from remaining in the material. For example, in some embodiments, voids do not remain in the material because they can escape as each layer is deposited. In some embodiments, a layer-by-layer process improves geometric homogeneity of the monomer reagent used.
[0169] In some embodiments, the polyphosphate foams disclosed herein can withstand high temperatures without formation of cracks or collapse of internal pores. In some embodiments, polyphosphate foams can withstand temperatures of up to 800 C., up to 900 C., or up to 1000 C. or any temperature in any range bounded by any value disclosed herein. In some embodiments, a polyphosphate foam can withstand a temperature of up to about 3000 C. for a short period of time (e.g., minutes to hours). In some embodiments, polyphosphate foams decompose at temperatures of at least 900 C. or at least 1000 C. over a prolonged period of time (e.g., days). In some embodiments, polyphosphate materials can withstand high temperatures because the OP bond in the backbone of polyphosphate materials is stable at high temperature. In some embodiments, polyphosphates can be used as flame retardants, optionally with additional additives such as ammonium phosphate.
[0170] In some embodiments, the polyphosphate foams disclosed herein can also withstand extremely low temperatures. In some embodiments, polyphosphate foams can withstand temperatures corresponding to that of liquid nitrogen. In some embodiments, polyphosphate foams can withstand temperatures of less than 0 C., 50 C., 60 C., 70 C., or 80 C., 100 C., 150 C., 180 C. or any temperature in any range bounded by any value disclosed herein. In some embodiments, polyphosphate foams can withstand temperatures of less than 0 C., 78 C. or 196C. In some embodiments, polyphosphate foams can withstand temperatures of less than 196 C.
[0171] In some embodiments, the polyphosphate foams disclosed herein have excellent mechanical properties. In some embodiments, phosphate materials can support over 250 times their own weight. In some embodiments, polyphosphate foams have a compressive strength of 100 to 200 kPa. In some embodiments, polyphosphate materials can sustain their mechanical properties across a range of temperatures, e.g., between room temperature and 600 C., as measured by dynamic mechanical analysis.
[0172] In some embodiments, polyphosphate foams can be stable in water. In some embodiments, polyphosphate foams do not degrade after weeks in water. The stability in water can be due to several factors, including the crystallinity or structural packing of the material, and the electrostatics (e.g., multivalency of the cation). In some embodiments, a passivation layer can form on the surface of a polyphosphate foam to protect the material from hydrolysis.
[0173] In some embodiments, polyphosphate foams can have a low thermal conductivity. In some embodiments, the thermal conductivity of a polyphosphate foam is about 0.01-0.05 W. m.sup.1.Math.K.sup.1.
[0174] In some embodiments, the polyphosphate foams disclosed herein can be good thermal insulators because they almost nullify heat transfer. First, in some embodiments, polyphosphate foams disclosed herein can reduce conduction of heat, for example, because they are highly porous and composed mostly of insulating gas. Second, in some embodiments, polyphosphate foams disclosed herein can reduce convection, for example, because the microstructure, including high porosity, prevents net gas movement. Super-insulating materials with low thermal conductivities are important for high temperature applications. Porous materials can have low thermal conductivity while also being ultralight. Porous materials can be good thermal insulators because they almost nullify two of the three methods of heat transfer: (1) conduction because they are mostly composed of insulating gas, (2) and convection because the porous microstructure prevents net gas movement. While the process and materials used to make super-insulating, porous materials are often expensive, the process and material to make polyphosphate foams is inexpensive.
[0175] In some embodiments, the polyphosphate foams disclosed herein have advantages over silica aerogels. Silica aerogels are synthesized by using a sol-gel process. Ethanol is mixed with a silicon alkoxide, such as tetramethoxysilane (TMOS), tetraethoxysilane (TEOS), and polyethoxydisiloxane (PEDS). The solution of silica is mixed with a catalyst and allowed to gel and form particles of silicon dioxide. The oxide suspension begins to undergo condensation reactions linking the dispersed colloidal particles. These reactions generally have moderately slow reaction rates, and as a result either acidic or basic catalysts are used to improve the processing speed. Basic catalysts tend to strengthen the material to prevent pore collapse during drying. Finally, during the drying process of the aerogel, the liquid surrounding the silica network is carefully removed and replaced with air (commercially, supercritical CO.sub.2 is used). Exemplary advantages of polyphosphate materials are as follows. First, for example, polyphosphate materials can have lower material costs than silica aerogels. Second, for example, while silica aerogels require an expensive process that includes freeze-drying, polyphosphate materials can be made using a low-cost process. Third, while silica aerogels use a freeze-drying process that takes days, polyphosphate materials can be made within seconds or minutes. Fourth, for example, while silica aerogels have only intermediate temperature resistance, polyphosphate materials have high temperature resistance and, in some embodiments, can withstand up to 2000 C. for minutes or withstand up to 900 C. for days. Fifth, for example, while silica aerogels are hydrophilic and have only intermediate water resistance, polyphosphate materials have high water resistance and, in some embodiments, can withstand for a month in water. Sixth, while silica aerogels are not biodegradable, polyphosphate materials can be biodegradable, and in some embodiments, degrade into biocompatible components.
[0176] In some embodiments, the polyphosphate foam can be a composite material that includes additional components. In some embodiments, additional components include nanomaterials. Exemplary nanomaterials include metal oxide nanoparticles, metal nanoparticles, metal nanorods, carbon fibers, clays, organic hybrids, silica, borosilicate, borate containing materials, and combinations thereof. Exemplary metal oxide nanoparticles include zirconia, titania, silica, alumina, zinc oxide, magnesium oxide, iron oxide, copper oxide, and combinations thereof. Exemplary metal nanoparticles or metal nanorods include gold nanoparticles, gold nanorods, silver nanoparticles, silver nanorods, copper nanoparticles, copper nanorods, and combinations thereof. Exemplary clays include Laponite, montmorillonite, kaolinite, and combinations thereof. In some embodiments, the additional components include metal oxides. Exemplary metal oxides include zirconia, titania, silica, alumina, zinc oxide, magnesium oxide, iron oxide, copper oxide, and combinations thereof.
[0177] In some embodiments, the polyphosphate foams disclosed herein can be used in various applications, for example, insulating materials, infrared masking materials, catalyst supports, and air purification, chemical adsorbers for cleaning up spills, fire-proof coatings, water purification, porous electrodes, or trapping space dust particles.
C. Fertilizers
[0178] In some embodiments, polyphosphate materials disclosed herein can be used as fertilizers. The transformation between monomer (orthophosphate) and polymer (polyphosphate) is fully reversible and free from side products except water. The simplicity of the polymerization and depolymerization processes can be useful in a circular economy, e.g., as fertilizers. For example, as shown
EXAMPLES
[0179] Certain embodiments will now be described in the following non-limiting examples.
I. Reversible Transformation Between Monomer and Polymer
[0180] Thermal polycondensation of potassium dihydrogen phosphate (KH.sub.2PO.sub.4) was performed.
II. Plasticized Polyphosphates
A. Preparing Amorphous Polyphosphates
[0181] To prepare amorphous polyphosphates, an equimolar mixture of sodium dihydrogen phosphate monohydrate (1.37 g, 10 mmol) and potassium dihydrogen phosphate (1.36 g, 10 mmol) was placed in a ceramic crucible and heated at 500 C. for 5 h in an oven to yield a quantitative amount of sodium-potassium (1:1) polyphosphate (Na/KPP) as a colorless liquid. The liquid was taken out of the oven and cooled to room temperature to give a colorless solid. The solid was ground into a fine powder.
[0182]
[0183]
B. Dissolution of Metal Salts in Polyphosphate Materials
[0184] Metal salts were dissolved in polyphosphate melts. In one example, 2.4 g of the Na/KPP powder and 170 mg (1.00 mmol) of CuCl.sub.3.Math.2H.sub.2O were placed in a glass vial and mixed with a vortex mixer. The mixture was heated with flame with gentle shaking until the solids melted and became a transparent liquid. Cooling the melt to room temperature furnished a blue-colored transparent solid.
[0185]
C. Polyphosphate Coacervates
[0186] To prepare a polyphosphate coacervatepotassium dihydrogen phosphate (100 g) was placed in a ceramic crucible and heated at 500 C. for 5 h in an oven to yield a quantitative amount of potassium polyphosphate (KPP) as a white solid. The solid was cooled to room temperature and ground into a fine powder. To a solution of sodium chloride (10.0 g) in water (150 mL), 20.0 g of the KPP (in powder form) was added portion by portion with vigorous stirring and kept stirred at room temperature for 7 h. The mixture was then boiled for 1.5 h to dissolve the powder. The suspension was cooled at 4 C. overnight, causing phase separation into two liquid layers. The lower layer is a coacervate of polyphosphate. The coacervate material can be a Na/K polyphosphate material where the KPP is dissolved by Na.sup.+ (from NaCl) via an ion exchange with keeping the polyphosphate from recrystallization. The high ion intensity of the solution induces phase separation to cause coacervation of the polyphosphate. Though, use of NaCl is for exemplary purposes only and can be replaced by other inorganic salts. Further, coacervate is composed mostly of the polyphosphate but contains water as well. The upper layer was removed by decantation.
[0187]
D. Polyphosphate Hydrogels
[0188] To prepare a polyphosphate hydrogel, 2.0 g of the polyphosphate coacervate described above was placed in a polystyrene container with 100 L of a 10 wt % dispersion of zinc oxide nanoparticles in water. The mixture was mixed by using a plastic spoon until gelling. The gel was subsequently kneaded with a powder-free latex glove until the gel surface was no longer sticky. In this example, the polyphosphate material can be a Na/KPP material. Though, the material can be a single or a combination of different cations.
[0189]
E. Polyphosphate Solutions and Coatings
[0190] To prepare polyphosphate coating, 200 mL of water was added to the polyphosphate coacervate (20 mL) and stirred at 4 C. overnight. A piece of filter paper (diameter: 5.5 cm) was dipped in the resultant solution. After removal of excess water with a piece of tissue paper, the polyphosphate-coated paper was dried in a desiccator under a reduced pressure. Though, a polyphosphate coating can also be formed using a melt or a solution. A Na/KPP material can be used to form the polyphosphate coating. Moreover, a solution of commercially available NaPP oligomers can also be used.
[0191]
F. Polyphosphate Adhesives
[0192] To prepare a polyphosphate adhesive, an equimolar mixture of sodium dihydrogen phosphate monohydrate (1.37 g, 10 mmol) and potassium dihydrogen phosphate (1.36 g, 10 mmol) was dissolved in 5 mL of water. 500 L of the solution was dropped onto the bottom (diameter: 2.7 cm) of an upside-down glass vial (weight: 1.4 g). The same procedure was repeated for a second glass vial. The two upside-down vials with the solution on the bottom were placed in a desiccator under a reduced pressure for 5 h to remove excess water. The vials were subsequently transferred into an oven. In the oven, one vial stood on the other vial that was upside-down, facing their bottoms. The pair of vials were heated at 500 C. for 5 h and then cooled to room temperature.
[0193]
[0194]
[0195]
[0196]
G. Polyphosphate Films
[0197] To form a polyphosphate film, a piece of Li/KPP solid was sandwiched with two sheets of Kapton (a polyimide film) and placed on an aluminum stage of a heat press machine. The solid was slowly pressed at 230 C. with increasing pressure and left at 3-10 atm (45-150 psi) at above 230 C. for 30 min. After cooling to room temperature, the pressure was released. The resulting polyphosphate film (flattened between the Kapton sheets) was taken out of the stage, and the Kapton sheets were peeled off from the polyphosphate film. Though, the provided pressure and temperature used are for example proposes only and can vary depending upon materials used.
[0198]
H. Hydrophobic Polyphosphate Materials
[0199]
III. Polyphosphate Foams
A. Preparing Polyphosphate Foams
[0200] Thermal polycondensation of aluminum dihydrogen phosphate led to the formation of a polyphosphate foam. The foam has density from 0.05 to 0.1 g/cm.sup.3.
B. Layer-by-Layer Fabrication of Polyphosphate Foams
[0201] Polyphosphate foams were formed using a layer-by-layer fabrication. Powdered aluminum dihydrogen phosphate was sprinkled onto a stainless-steel plate. The steel plate can be 20 cm20 cm0.3 cm. It was followed by heating the layer of powder by blowing a flame from the top using a MAPP gas torch at a temperature around 2050 C. Though, the temperature is for example purposes only and can vary (e.g., between 500 C. to 2900 C.) The powder was heated until foaming stopped. This procedure was repeated to make a monolithic block of aluminum polyphosphate (AlPP) foam layer by layer. The resulting PP monolith was cut into a desired shape by using a razor or a CO.sub.2 laser cutter (10,600 nm, 35 W).
[0202]
C. Mechanical Stability of Polyphosphate Foams
[0203]
D. Absorbance of Polyphosphate Foams
[0204] As shown in
[0205] As shown in
E. Thermal Insulation by Polyphosphate Foams
[0206] As shown in
[0207]
[0208] Preliminary results show that thermal conductivity of polyphosphate form at room temperature is about 0.03 W.Math.m.sup.1.Math.K.sup.1. This value is comparable to reported values of polyurethane foam (0.05 W.Math.m.sup.1.Math.K.sup.1) and silica aerogel (0.02 W.Math.m.sup.1.Math.K.sup.1). The thermal stability of polyphosphate foam is much higher than those common insulating materials, making polyphosphate foam useful for thermal insulation at extreme temperatures.
[0209] Table 1 shows a comparison of polyphosphate foams with silica aerogels and other insulating materials. As shown in Table 1, polyphosphate foams can withstand a wider range of temperatures.
TABLE-US-00001 TABLE 1 Comparison of Polyphosphate foams with other insulators. Optimal thermal Thermal performance Conductivity Density Polyphosphate 70 C. to 800 C. 0.03 W .Math. m.sup.1 .Math. K.sup.1 0.05-0.15 g/cm.sup.3 foams CRYOGEL x201 Up to 200 C. 0.017 W .Math. m.sup.1 .Math. K.sup.1 0.13 g/cm.sup.3 (Aspen Aerogels) PYROGEL HPS Up to 650 C. 0.022 W .Math. m.sup.1 .Math. K.sup.1 0.20 g/cm.sup.3 (Aspen Aerogels) Lumira Aerogel Up to 300 C. 0.018 W .Math. m.sup.1 .Math. K.sup.1 0.12-0.15 g/cm.sup.3 (Cabot) SpaceLoft Subsea Up to 200 C. 0.0145 W .Math. m.sup.1 .Math. K.sup.1 0.16 g/cm.sup.3 (Aspen Aerogels) Polyurethane Up to 80 C. 0.05 W .Math. m.sup.1 .Math. K.sup.1 0.1 g/cm.sup.3 Insulation Styrofoam Up to 100 C. 0.033 W .Math. m.sup.1 .Math. K.sup.1 0.05 g/cm.sup.3
F. Thermal Degradation of Polyphosphate Foams
[0210]
[0211] A porous monolith of AlPP was heated at 2000 C. (with a MAPP gas torch) for 10 min and analyzed by powder X-ray diffraction (XRD) analysis. The diffractogram, shown in
G. Stability of Polyphosphate Foam in Water
[0212] In some embodiments, the degradation can be further reduced by making polyphosphate foams hydrophobic via a chemical treatment. Further, the surface of AlPP foams can be hydrophobized via ion exchange. For example, sodium dodecyl sulfate can be introduced on the surface to delay the hydrolytic degradation.
[0213]
H. Polyphosphate Foam Composites
[0214]
IV. Polyphosphate Fertilizers
[0215] Used polyphosphate materials can be reused as fertilizer. As shown in
[0216] As shown in
[0217] It will be appreciated that while one or more particular materials or steps have been shown and described for purposes of explanation, the materials or steps may be varied in certain respects, or materials or steps may be combined, while still obtaining the desired outcome. Additionally, modifications to the disclosed embodiment and the invention as claimed are possible and within the scope of this disclosed invention.
[0218] The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the disclosure. As used herein, the singular forms a, an and the are intended to include the plural forms as well, unless the context clearly indicates otherwise. It will be further understood that the terms comprises and/or comprising, when used in this specification, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof.