# US 10,767,009 B2 · Process for preparing polyether polyol using DMC catalyst and continuous addition of starter

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- Number: US 10,767,009 B2
- Document ID: US10767009B2
- Status: Granted
- Kind: B2
- Application number: 15/737,813
- Filed: 2016-06-20
- Published: 2018-08-23
- Granted: 2020-09-08
- Earliest claimed: 2015-07-02
- Assignees: Covestro LLC
- Applicants: Covestro LLC
- Inventors: Jean-Paul Masy; Carlos M. Villa; David A. Babb; John W. Weston; Sweta Somasi
- Web page: https://patentgrep.com/patent/US10767009B2

## CPC

- C08G 65/2663: {Metal cyanide catalysts, i.e. DMC's}
- C08G 18/4829: {Polyethers containing at least three hydroxy groups (C08G18/4833 - C08G18/5096 take precedence)}
- C08G 65/2696: {characterised by the process or apparatus used}
- C08G 2110/0025: rigid
- C08G: MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS

## Abstract

Polyether polyols are made by a process that includes a continuous addition of starter and alkylene oxide. The feed of starter is discontinued when 80 to 95% of the alkylene oxide has been fed to the reactor. This process produces a product with a narrow molecular weight distribution.

## Claims

### Claim 1

A process for making a polyether polyol product, comprising:
a) activating a DMC catalyst complex in the presence of i) an alkoxylated starter having a hydroxyl equivalent weight of 50 to 100% of the hydroxyl equivalent weight of the polyether polyol product and ii) up to 10 weight-%, based on the weight of the alkoxylated starter, of 1,2-propylene oxide;
b) continuously feeding an alkylene oxide containing at least 50 weight-% 1,2-propylene oxide to the activated DMC catalyst under polymerization conditions,
wherein starting at the beginning of step b), a low equivalent weight starter is fed continuously to the activated DMC catalyst under polymerization conditions, the feed of low molecular weight starter is continued until 80 to 95% of the alkylene oxide feed in step b) has been completed and the feed of low molecular weight starter is then discontinued while continuing the alkylene oxide feed, wherein the total weight of low molecular weight starter added in step b) is 0.2 to 25% of the total weight of alkylene oxide added in step b).

### Claim 2 (depends on 1)

The process of claim 1 wherein in step b), the feed of low molecular weight starter is continued until 81 to 90% of the alkylene oxide feed in step b) has been completed.

### Claim 3 (depends on 1)

The process of claim 1 wherein in step b), the low molecular weight starter and alkylene oxide are fed at a constant ratio until the feed of low molecular weight starter is discontinued.

### Claim 4 (depends on 1)

The process of claim 1, wherein the alkylene oxide is 1,2-propylene oxide.

### Claim 5 (depends on 1)

The process of claim 1, wherein the low molecular weight starter is propylene glycol.

### Claim 6 (depends on 1)

The process of claim 1, wherein the polyether polyol product has a hydroxyl equivalent weight of 350 to 750 and a nominal functionality of 2 to 4.

### Claim 7

A polyether polyol comprising the reaction product of
a) an activated DMC catalyst complex in the presence of i) an alkoxylated starter having a hydroxyl equivalent weight of 50 to 100% of the hydroxyl equivalent weight of the polyether polyol product and ii) up to 10 weight %, based on the weight of the alkoxylated starter, of 1,2-propylene oxide;
with
b) an alkylene oxide comprising at least 50 weight % of 1,2-propylene oxide, with said alkylene oxide being continuously fed to said activated DMC catalyst complex under polymerization conditions;
and
c) a low molecular weight starter which is continuously fed to said activated DMC catalyst under polymerization conditions at the beginning of feeding said alkylene oxide b);
wherein the feed of said low molecular weight starter is continued until 80 to 95% of the feed of said alkylene oxide b) is completed and the feed of low molecular weight starter is then discontinued while continuing the feed of said alkylene oxide b), wherein the total weight of low molecular weight starter added during the feed of said alkylene oxide is 0.2 to 25% of the total weight of the feed of said alkylene oxide b).

### Claim 8

A polyether polyol containing double metal catalyst residues, having a number average hydroxyl equivalent weight of 500 to 2000, and a molecular weight distribution, as determined by gel permeation chromatography, with a peak molecular weight wherein less than 1 weight percent of molecules have a molecular weight of 140% or more than the peak molecular weight, and less than 1 weight percent of molecules have a molecular weight of 65% or less of the peak molecular weight.

### Claim 9 (depends on 7)

A formulated polyol composition comprising the polyether polyol of claim 7, water, and 5 to 40% by weight, based on the weight of the formulated polyol composition, of at least one physical blowing agent.

### Claim 10 (depends on 9)

The formulated polyol composition of claim 9 which comprises 5 to 50% of said polyether polyol, based on the total weight of the formulated polyol composition, 1.5 to 4% of water, based on the total weight of the formulated polyol composition, and said physical blowing agent comprises cyclopentane.

### Claim 11 (depends on 7)

The polyether polyol of claim 7, wherein the feed of said low molecular weight starter is continued until 80 to 92% of the feed of said alkylene oxide b) is completed and the feed of low molecular weight starter is then discontinued while continuing the feed of said alkylene oxide b).

### Claim 12 (depends on 7)

The polyether polyol of claim 7, wherein the feed of said low molecular weight starter is continued until 81 to 90% of the feed of said alkylene oxide b) is completed and the feed of low molecular weight starter is then discontinued while continuing the feed of said alkylene oxide b).

### Claim 13 (depends on 8)

A formulated polyol composition comprising the polyether polyol of claim 8, water, and 5 to 40% by weight, based on the weight of the formulated polyol composition, of at least one physical blowing agent.

### Claim 14 (depends on 13)

The formulated polyol composition of claim 13 which comprises 5 to 50% of said polyether polyol, based on the total weight of the formulated polyol composition, 1.5 to 4% of water, based on the total weight of the formulated polyol composition, and said physical blowing agent comprises cyclopentane.