Aqueous cationic polyurethane dispersions
US-9527328-B2 · Dec 27, 2016 · US
US9828459B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-9828459-B2 |
| Application number | US-201514823588-A |
| Country | US |
| Kind code | B2 |
| Filing date | Aug 11, 2015 |
| Priority date | Aug 11, 2015 |
| Publication date | Nov 28, 2017 |
| Grant date | Nov 28, 2017 |
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A continuous process for preparing a silylated polymer comprising a silylation step where a prepolymer having reactive functional groups, a first intermediate product, is reacted continuously with a silylating agent in an endcapping tubular reaction unit to form a second intermediate product, and where at least a portion of the second intermediate product is backmixed continuously with the first intermediate product to form the silylated polymer. The continuous process may further comprise a stabilization step, a quenching step or both a stabilization step and a quenching step.
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The invention claimed is: 1. A process for the preparation of a silylated polymer comprising continuously reacting a prepolymer with a silylating agent, by a silylation reaction, to produce a silylated polymer composition; and continuously backmixing at least a first portion of the silylated polymer composition with a loop connected from a downstream outlet to an upstream outlet of a reactor to adjust at least one upstream process parameter. 2. The process of claim 1 , wherein the silylated polymer composition comprises a fully silylated polymer and a partially silylated polymer. 3. The process of claim 1 , wherein a weight ratio of the first portion of the silylated polymer composition to the prepolymer ranges from about 0.05:1 to about 5:1. 4. The process of claim 1 , wherein the at least one upstream process parameter is at least one of residence time, temperature, weight ratio of the first portion to the prepolymer. 5. The process of claim 1 , wherein the prepolymer is a polyol with reactive functional groups or a chain extended prepolymer with reactive functional groups. 6. The process of claim 5 , wherein the reactive functional groups of either or both of the polyol and chain extended polymer are terminal reactive functional groups. 7. The process of claim 5 , wherein the chain extended prepolymer is prepared by continuously reacting a polyol with a chain extension agent. 8. The process of claim 1 further comprising continuously reacting at least a second portion of the silylated polymer composition with a scavenging agent or scavenging package to produce a quenched silylated polymer composition. 9. The process of claim 7 , wherein the chain extension agent is a diisocyanate or a polyisocyanate. 10. The process of claim 6 , wherein the terminal reactive functional groups are at least one of hydroxyl or isocyanate. 11. The process of claim 1 , wherein the silylating agent is an isocyanatosilane, mercaptosilane, hydroxyl-functional silane or an aminosilane. 12. The process of claim 1 , wherein the silylated polymer composition comprises a moisture-curable silylated polyurethane polymer. 13. The process of claim 8 , wherein the scavenging package comprises at least one cyclic amide scavenging agent. 14. The process of claim 13 , wherein the scavenging package further comprises a vinyltrimethoxysilane in a blend with the at least one cyclic amide scavenging agent. 15. The process of claim 13 , wherein the cyclic amide is selected from the group consisting of ε-caprolactam, 2-pyrrolidone and combinations thereof. 16. The process of claim 6 , wherein at least one of the terminal reactive functional groups is isocyanate and the silylating agent is an aminosilane. 17. The process of claim 6 , wherein at least one of the terminal reactive functional groups is a hydroxyl group and the silylating agent is an isocyanatosilane. 18. The process of claim 1 , further comprising adding a stabilization package to the process. 19. The process of claim 18 , wherein the stabilization package comprises at least one of a hindered phenol or phosphite stabilizer. 20. The process of claim 14 further comprising a stabilization package having triisodecyl phosphite.
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