Process for preparing polyoxymethylene

Patent metadata

Field	Value
Publication number	US-9765172-B2
Application number	US-201414894158-A
Country	US
Kind code	B2
Filing date	May 26, 2014
Priority date	May 29, 2013
Publication date	Sep 19, 2017
Grant date	Sep 19, 2017

Abstract

The patent application relates to a process for preparing polyoxymethylene by polymerization of a reaction mixture (R G ) which comprises at least one formaldehyde source and at least one initiator mixture (I G ), wherein the initiator mixture (I G ) comprises at least one polymerization initiator and at least one solvent of the general formula (I)

R 1 —O—[—R 3 —O—] m —R 2   (I),
where m is 1, 2, 3 or 4; R 1 and R 2 are each, independently of one another, C 3 -C 6 -alkyl; R 3 is C 1 -C 5 -alkylene.

First claim

The invention claimed is:

1. A process for preparing polyoxymethylene, comprising polymerizing a reaction mixture (R G ) which comprises a formaldehyde source and an initiator mixture (I G ), wherein the initiator mixture (I G ) comprises a polymerization initiator and a solvent of formula (I):
R 1 —O—[—R 3 —O—] m —R 2   (I),

wherein
m is 1, 2, 3 or 4;
R 1 and R 2 are each, independently of one another, C 3 -C 6 -alkyl; and
R 3 is ethylene.

2. The process according to claim 1 , wherein the formaldehyde source is selected from the group consisting of cyclic and linear formals.

3. The process according to claim 1 , wherein
m is 1, 2, 3 or 4; and
R 1 and R 2 are both unsubstituted C 3 -C 6 -alkyl.

4. The process according to claim 1 , wherein the reaction mixture (R G ) further comprises a first comonomer (C-1).

5. The process according to claim 4 , wherein the comonomer (C-1) is a cyclic ether of formula (II):

wherein
R 11 to R 14 are each, independently of one another, H, C 1 -C 4 -alkyl or halogen-substituted C 1 -C 4 -alkyl;
R 15 is a chemical bond, a (—CR 15a R 15b —) group or a (—CR 15a R 15b O—) group, where R 15a and R 15b are each, independently of one another, H, unsubstituted or at least monosubstituted C 1 -C 4 -alkyl in which the substituents are selected from among F, Cl, Br, OH and C 1 -C 4 -alkyl; and
n is 0, 1, 2 or 3.

6. The process according to claim 4 , wherein the reaction mixture (R G ) comprises up to 50 mol %, based on the formaldehyde source, of the comonomer (C-1).

7. The process according to claim 1 , wherein the polymerization initiator is a protic acid or a Lewis acid.

8. The process according to claim 1 , wherein the polymerization initiator is added in an amount of from 0.0001 ppm to 1000 ppm, based on the reaction mixture (R G ).

9. The process according to claim 1 , wherein the polymerization initiator is dissolved in the solvent (I) in a concentration of from 0.005% by weight to 5% by weight, based on a total weight of the initiator mixture (I G ).

10. The process according to claim 1 , wherein the reaction mixture (R G ) further comprises a chain transfer agent.

11. The process according to claim 10 , wherein the chain transfer agent is added in an amount of from 10 ppm to 10 000 ppm, based on the reaction mixture (R G ).

12. The process according to claim 1 , wherein the reaction mixture (R G ) further comprises a second comonomer (C-2), which is a bifunctional compound of formula (III) or (IV):

wherein
Z is a chemical bond, an (—O—) group or an (—O—R 21 —O—) group, where R 21 is unsubstituted C 1 -C 8 -alkylene or C 3 -C 8 -cycloalkylene.

13. The process of claim 1 , further comprising dissolving the polymerization initiator in the solvent of formula (I) in a concentration of from 0.005% by weight to 5% by weight.

14. The process of claim 1 , wherein solvent in the initiator mixture consists essentially of at least one solvent of formula (I).

15. The process of claim 1 , wherein the solvent of formula (I) is diethylene glycol dipropyl ether, diethylene glycol dibutyl ether, diethylene glycol dipentyl ether, or diethylene glycol dihexyl ether, or any mixture thereof.

16. The process of claim 1 , wherein the solvent of formula (I) is diethylene glycol dibutyl ether.

17. The process of claim 1 , wherein R 1 and R 2 are each, independently of one another, linear C 3 -C 6 -alkyl.

18. A process for preparing polyoxymethylene, comprising polymerizing a reaction mixture (R G ) which comprises a formaldehyde source and an initiator mixture (I G ), wherein the initiator mixture (I G ) comprises a polymerization initiator and a solvent of formula (I):
R 1 —O—[—R 3 —O—] m —R 2   (I),

wherein
m is 1, 2, 3 or 4;
R 1 and R 2 are each, independently of one another, C 3 -C 6 -alkyl; and
R 3 is ethylene, and
wherein a degree of solvent migration is less than 10 μg/kg.

Assignees

• Basf Se

Inventors

• Pottie Laurence
• Demeter Juergen
• Hermant Marie-Claire

Classifications

• C08G2/10 Primary

  Polymerisation of cyclic oligomers of formaldehyde · CPC title

• C08G65/00

  Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule · CPC title

• C08G2/22

  with epoxy compounds · CPC title

• C08G4/00

  Condensation polymers of aldehydes or ketones with polyalcohols; Addition polymers of heterocyclic oxygen compounds containing in the ring at least once the grouping —O—C—O— (of cyclic oligomers of aldehydes C08G2/00) · CPC title

• C08L59/04

  Copolyoxymethylenes · CPC title