Purification of polyols prepared using double metal cyanide complex catalysts

Claim 2

A process for purifying a polyol containing a double metal cyanide complex catalyst which comprises the steps of: (a) treating the polyol with at least one alkali metal compound selected from the group consisting of alkali metals, alkali metal hydroxides, alkali metal hydrides, and alkali metal alkoxides in an amount sufficient to convert the double metal cyanide complex catalyst into an insoluble portion and a soluble portion and to convert at least a portion of the polyol hydroxyl groups to alkoxide groups, (b) filtering the treated polyol to remove the insoluble portion, (c) further treating the filtered polyol with a sufficient amount of at least one phosphorous compound to convert the soluble portion of the double metal cyanide complex catalyst produced in step (a) to a second insoluble portion, said phosphorous compound selected from the group consisting of pyrophosphorous acid, hypophosphorous acid, phosphorous acid, and compounds having the formula ##STR1## wherein R is linear or branched alkyl, phenyl, or substituted phenyl, X is Cl or Br, x is 0, 1, 2, or 3, y is 0, 1, or 2, z is 0, 1, 2, or 3, and the sum of x+y+z is 3, with the proviso that the filtered polyol additionally be treated with water when the phosphorous compound is pyrophosphorous acid or when x is 1, 2, or 3, or z is 1, 2, or 3, (d) filtering the phosphorous compound-treated polyol to remove the second insoluble portion of the double metal cyanide complex catalyst produced in step (c), and (e) recovering the resulting purified polyol

Claim 3

The process of claim 1 wherein the phosphorous compound is hypophosphorous acid.

Claim 4

The process of claim 1 wherein the phosphorous compound is phosphorous acid.

Claim 5

The process of claim 1 wherein step (b) is performed in the presence of a filter aid.

Claim 6

The process of claim 1 wherein step (d) is performed in the presence of a filter aid.

Claim 7

The process of claim 1 wherein the double metal cyanide complex catalyst is a zinc hexacyanocobaltate complex catalyst.

Claim 8

The process of claim 1 wherein the polyol is poly(propylene glycol).

Claim 9

The process of claim 1 wherein the polyol is a random copolymer of propylene oxide and ethylene oxide.

Claim 10

The process of claim 1 wherein the alkali metal compound is potassium hydroxide.

Claim 11

The process of claim 1 wherein the alkali metal compound is sodium methoxide.

Claim 12

The process of claim 1 wherein the alkali metal compound is sodium metal.

Claim 13

The process of claim 1, comprising the additional step of contacting the polyol after step (a) and before step (b) with an adsorbent agent in an amount sufficient to adsorb any excess of the alkali metal compound and to convert the polyol alkoxide groups to hydroxyl groups.

Claim 14

The process of claim 1, comprising the additional step of contacting the polyol after step (c) and before step (d) with an adsorbent agent in an amount sufficient to adsorb any excess of the phosphorous compound.

Claim 15

The process of claim 1, comprising the additional step of contacting the polyol with ethylene oxide after step (a) and before step (b) in an amount sufficient to form an ethylene oxide-capped polyol having a substantial portion of hydroxyl end groups which are primary.

Claim 16

A process for purifying a polyol containing a double metal cyanide complex catalyst which comprises the steps of: (a) treating the polyol with at least one alkali metal compound selected from the group consisting of alkali metals, alkali metal hydroxides, alkali metal hydrides, and alkali metal alkoxides in an amount sufficient to convert the double metal cyanide complex catalyst into a first insoluble portion and a soluble portion and to convert at least a portion of the polyol hydroxyl groups to alkoxide groups, (b) further treating the polyol obtained in step (a) with a sufficient amount of at least one phosphorous compound to convert the soluble portion of the double metal cyanide complex catalyst to a second insoluble portion, said phosphorous compound selected form the group consisting of pyrophosphorous acid, hypophosphorous acid, phosphorous acid, and compounds having the formula ##STR2## wherein R is linear or branched alkyl, phenyl, or substituted phenyl, X is Cl or Br, x is 0, 1, 2, or 3, y is 0, 1, or 2, z is 0, 1, 2, or 3, and the sum of x+y+z is 3, with the proviso that the filtered polyol additionally be treated with water when the phosphorous compound is pyrophosphorous acid or when x is 1, 2, or 3 or when z is 1, 2, or 3, (c) filtering the treated polyol to remove the first and second insoluble portions of the double metal cyanide complex catalyst, and (d) recovering the resulting purified polyol.

Claim 17

A process for purifying a polyol containing a double metal cyanide complex catalyst which comprises the steps of: (a) treating the polyol with at least one alkali metal compound selected from the group consisting of alkali metals, alkali metal hydroxides, alkali metal hydrides, and alkali metal alkoxides in an amount sufficient to convert the double metal cyanide complex catalyst into a first insoluble portion and a soluble portion and to convert at least a portion of the polyol hydroxyl groups to alkoxide groups, (b) further treating the polyol obtained in step (a) with a sufficient amount of at least one phosphorous compound to convert the soluble portion of the double metal cyanide complex catalyst to a second insoluble portion, said phosphorous compound selected form the group consisting of pyrophosphorous acid, hypophosphorous acid, phosphorous acid, and compounds having the formula ##STR2## wherein R is linear or branched alkyl, phenyl, or substituted phenyl, X is Cl or Br, x is 0, 1, 2, or 3, y is 0, 1, or 2, z is 0, 1, 2, or 3, and the sum of x+y+z is 3, with the proviso that the filtered polyol additionally be treated with water when the phosphorous compound is pyrophosphorous acid or when x is 1, 2, or 3 or when z is 1, 2, or 3, (c) filtering the treated polyol to remove the first and second insoluble portions of the double metal cyanide complex catalyst, and (d) recovering the resulting purified polyol.

Claim 18

The process of claim 15 wherein the phosphorous compound is hypophosphorous acid.

Claim 19

The process of claim 15 wherein the phosphorous compound is phosphorous acid.

Claim 20

The process of claim 15 wherein step (c) is performed in the presence of a filter aid.

Claim 21

The process of claim 15 wherein the double metal cyanide complex catalyst is a zinc hexacyanocobaltate complex catalyst.

Claim 22

The process of claim 15 wherein the polyol is poly(propylene glycol).

Claim 23

The process of claim 15 wherein the polyol is a random copolymer of propylene oxide and ethylene oxide.

Claim 24

The process of claim 15 wherein the alkali metal compound is potassium hydroxide.

Claim 25

The process of claim 15 wherein the alkali metal compound is sodium methoxide.

Claim 26

The process of claim 15 wherein the alkali metal compound is sodium metal.

Claim 27

The process of claim 15, comprising the additional step of contacting the polyol after step (b) and before step (c) with at least one adsorbent agent in an amount sufficient to adsorb any excess of the alkali metal compound, convert the polyol alkoxide groups to hydroxyl groups, and adsorb any excess of the phosphorous compound.

Claim 28

The process of claim 15, comprising the additional step of contacting the polyol with ethylene oxide after step (a) and before step (b) in an amount sufficient to form an ethylene oxide-capped polyol having a substantial portion of hydroxyl and groups which are primary.

Claim 29

A process for purifying a polyol containing a double metal cyanide complex catalyst which comprises the steps of: (a) treating the polyol with at least one metal compound selected from the group consisting of alkali metals, alkali metal hydroxides, alkali metal hydrides, and alkali metal alkoxides in an amount sufficient to convert the double metal cyanide complex catalyst into an insoluble portion and a soluble portion and to convert at least a portion of the polyol hydroxyl groups to alkoxide groups, (b) contact the treated polyol with a first adsorbent agent in an amount sufficient to adsorb any excess of the alkali metal compound and to convert the polyol alkoxide groups to hydroxyl groups, (c) filtering the polyol to remove the insoluble portion of the double metal cyanide complex catalyst and the adsorbent agent containing adsorbed excess alkali metal compound, (d) treating the filtered polyol with a phosphorous compound selected from the group consisting of hypophosphorous acid and phosphorous acid in an amount sufficient to convert the soluble portion of the double metal cyanide complex catalyst to a second insoluble portion, (e) contacting the polyol with a second adsorbent agent in an amount sufficient to adsorb any excess of the phosphorous compound, (f) filtering the polyol to remove the second insoluble portion of the double metal cyanide complex catalyst and the second adsorbent agent containing adsorbed excess phosphorous compound, and (g) recovering the resulting purified polyol.

Claim 30

A process for purifying a polyol containing a double metal cyanide complex catalyst which comprises the steps of: (a) treating the polyol with at least one metal compound selected from the group consisting of alkali metals, alkali metal hydroxides, alkali metal hydrides, and alkali metal alkoxides in an amount sufficient to convert the double metal cyanide complex catalyst into an insoluble portion and a soluble portion and to convert at least a portion of the polyol hydroxyl groups to alkoxide groups, (b) contact the treated polyol with a first adsorbent agent in an amount sufficient to adsorb any excess of the alkali metal compound and to convert the polyol alkoxide groups to hydroxyl groups, (c) filtering the polyol to remove the insoluble portion of the double metal cyanide complex catalyst and the adsorbent agent containing adsorbed excess alkali metal compound, (d) treating the filtered polyol with a phosphorous compound selected from the group consisting of hypophosphorous acid and phosphorous acid in an amount sufficient to convert the soluble portion of the double metal cyanide complex catalyst to a second insoluble portion, (e) contacting the polyol with a second adsorbent agent in an amount sufficient to adsorb any excess of the phosphorous compound, (f) filtering the polyol to remove the second insoluble portion of the double metal cyanide complex catalyst and the second adsorbent agent containing adsorbed excess phosphorous compound, and (g) recovering the resulting purified polyol.

Claim 31

The process of claim 27 wherein step (c) is performed in the presence of a filter aid.

Claim 32

The process of claim 27 wherein step (f) is performed in the presence of a filter aid.

Claim 33

The process of claim 27 wherein the double metal cyanide complex catalyst is a zinc hexacyanocobaltate complex catalyst.

Claim 34

The process of claim 27 wherein the polyol is poly(propylene glycol).

Claim 35

The process of claim 27 wherein the polyol is a random copolymer of propylene oxide and ethylene oxide.

Claim 36

The process of claim 27 wherein the alkali metal compound is potassium hydroxide.

Claim 37

The process of claim 27 wherein the alkali metal compound is sodium methoxide.

Claim 38

The process of claim 27 wherein the alkali metal compound is sodium metal.

Claim 39

The process of claim 27, comprising the additional step of contacting the polyol with ethylene oxide after step (a) and before step (b) in an amount sufficient to form an ethylene oxide-capped polyol having a substantial portion of hydroxyl end groups which are primary.

Claim 40

A process for purifying poly(propylene glycol) containing a zinc hexacyanocobaltate complex catalyst which comprises the steps of: (a) treating the poly(propylene glycol) with at least one alkali metal compound selected from the group consisting of sodium metal, potassium hydroxide, and sodium methoxide in an amount sufficient to convert the zinc hexacyanocobaltate complex catalyst into an insoluble portion and a soluble portion and to convert at least a portion of the poly(propylene glycol) hydroxyl groups to alkoxide groups, (b) contacting the treated poly(propylene glycol) with magnesium silicate in an amount sufficient to adsorb any excess of the alkali metal compound and to convert the poly(propylene glycol) alkoxide groups to hydroxyl groups, (c) filtering the poly(propylene glycol) in the presence of a filter aid to remove the insoluble portion of the zinc hexacyanocobaltate complex catalyst and the magnesium silicate containing adsorbed excess alkali metal compound, (d) treating the filtered poly(propylene glycol) with a phosphorous compound selected from the group consisting of hypophosphorous acid and phosphorous acid in an amount sufficient to convert the soluble portion of the zinc hexacyanocobaltate complex catalyst to a second insoluble portion, e) contacting the poly(propylene glycol) with additional magnesium silicate in an amount sufficient to adsorb any excess of the phosphorous compound, (f) filtering the poly(propylene glycol) in the presence of a filter aid to remove the second insoluble portion of the zinc hexacyanocobaltate complex catalyst and the additional magnesium silicate containing adsorbed excess phosphorous compound, and (g) recovering the resulting purified poly(propylene glycol).

Claim 41

A process for purifying poly(propylene glycol) containing a zinc hexacyanocobaltate complex catalyst which comprises the steps of: (a) treating the poly(propylene glycol) with at least one alkali metal compound selected from the group consisting of sodium metal, potassium hydroxide, and sodium methoxide in an amount sufficient to convert the zinc hexacyanocobaltate complex catalyst into an insoluble portion and a soluble portion and to convert at least a portion of the poly(propylene glycol) hydroxyl groups to alkoxide groups, (b) contacting the treated poly(propylene glycol) with magnesium silicate in an amount sufficient to adsorb any excess of the alkali metal compound and to convert the poly(propylene glycol) alkoxide groups to hydroxyl groups, (c) filtering the poly(propylene glycol) in the presence of a filter aid to remove the insoluble portion of the zinc hexacyanocobaltate complex catalyst and the magnesium silicate containing adsorbed excess alkali metal compound, (d) treating the filtered poly(propylene glycol) with a phosphorous compound selected from the group consisting of hypophosphorous acid and phosphorous acid in an amount sufficient to convert the soluble portion of the zinc hexacyanocobaltate complex catalyst to a second insoluble portion, e) contacting the poly(propylene glycol) with additional magnesium silicate in an amount sufficient to adsorb any excess of the phosphorous compound, (f) filtering the poly(propylene glycol) in the presence of a filter aid to remove the second insoluble portion of the zinc hexacyanocobaltate complex catalyst and the additional magnesium silicate containing adsorbed excess phosphorous compound, and (g) recovering the resulting purified poly(propylene glycol).

Claim 42

The process of claim 27, comprising the additional step of contacting the poly(propylene glycol) with ethylene oxide after step (a) and before step (b) in an amount sufficient to form an ethylene oxide-capped poly(propylene glycol) having a substantial portion of hydroxy end groups which are primary.