# US 10,308,772 B2 · Method for producing pseudopolyrotaxane aqueous dispersion

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- Number: US 10,308,772 B2
- Document ID: US10308772B2
- Status: Granted
- Kind: B2
- Application number: 15/540,520
- Filed: 2016-01-08
- Published: 2017-12-07
- Granted: 2019-06-04
- Earliest claimed: 2015-01-09
- Assignees: Sumitomo Seika Chemicals Co., Ltd.; Advanced Softmaterials Inc.
- Applicants: Sumitomo Seika Chemicals Co., Ltd.
- Inventors: Naohisa Hayamizu; Hiroki Okazaki; Akira Kimura; Shinya Okazaki
- Web page: https://patentgrep.com/patent/US10308772B2

## CPC

- C08J 3/03: in aqueous media
- B82Y 5/00: Nanobiotechnology or nanomedicine, e.g. protein engineering or drug delivery
- C08B 37/0015: {Inclusion compounds, i.e. host-guest compounds, e.g. polyrotaxanes}
- C08G 83/007: {Polyrotaxanes; Polycatenanes}
- C08J 3/005: {Processes for mixing polymers}
- C08L 5/16: Cyclodextrin; Derivatives thereof
- C08L 71/02: Polyalkylene oxides
- C08G 2650/04: End-capping
- C08J: WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H (working, e.g. shaping, of plastics B29)
- B82Y: SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- C08B: POLYSACCHARIDES; DERIVATIVES THEREOF (polysaccharides containing less than six saccharide radicals attached to each other by glycosidic linkages C07H; fermentation or enzyme-using processes C12P19/00; sugar industry C13; production of cellulose D21)
- C08G: MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08L: COMPOSITIONS OF MACROMOLECULAR COMPOUNDS (compositions based on polymerisable monomers C08F, C08G; artificial filaments or fibres D01F; textile treating compositions D06)

## Abstract

The present invention provides a method for producing an aqueous dispersion of pseudopolyrotaxane that enables the production, by an industrially advantageous method for an aqueous dispersion of pseudopolyrotaxane in which the inclusion amount of a cyclodextrin does not increase with time and which can provide a crosslinked polyrotaxane having sufficient stretchability and breaking strength. The present invention relates to a method for producing an aqueous dispersion of pseudopolyrotaxane containing pseudopolyrotaxane particles in which a polyethylene glycol is included in a cavity of a cyclodextrin molecule in a skewered manner, the method including: an inclusion step of mixing a polyethylene glycol and a cyclodextrin in an aqueous medium to include the polyethylene glycol in a cavity of a cyclodextrin molecule, wherein in the inclusion step, a basic compound is added.

## Claims

### Claim 1

A method for producing an aqueous dispersion of a pseudopolyrotaxane containing pseudopolyrotaxane particles in which a polyethylene glycol is included in a cavity of a cyclodextrin molecule in a skewered manner,
the method comprising:
an inclusion step of mixing the polyethylene glycol and a molecular cyclodextrin in an aqueous medium to include the polyethylene glycol in the cavity of the cyclodextrin molecule,
wherein the inclusion step includes a mixing step of dissolving the polyethylene glycol and the cyclodextrin in the aqueous medium to prepare a mixed solution, and a cooling step of cooling the mixed solution to precipitate pseudopolyrotaxane particles, and
a basic compound is added after the pseudopolyrotaxane has been precipitated in the cooling step.

### Claim 2 (depends on 1)

The method for producing the aqueous dispersion of the pseudopolyrotaxane according to claim 1,
wherein the basic compound is added in an amount of 0.1 to 10 times the number of moles of reactive groups at both ends of the polyethylene glycol.

### Claim 3 (depends on 1)

The method for producing the aqueous dispersion of the pseudopolyrotaxane according to claim 1,
wherein the polyethylene glycol has a mass average molecular weight of 1,000 to 100,000.

### Claim 4 (depends on 1)

The method for producing the aqueous dispersion of the pseudopolyrotaxane according to claim 1,
wherein a mass ratio of the polyethylene glycol and the cyclodextrin is 1:2 to 1:5.

### Claim 5 (depends on 1)

A method for producing a polyrotaxane containing a cyclodextrin, a polyethylene glycol included in a cavity of the cyclodextrin in a skewered manner, and capping groups at both ends of the polyethylene glycol,
the method comprising the steps of:
producing an aqueous dispersion of a pseudopolyrotaxane by the production method according to claim 1, and
introducing capping groups in an aqueous medium constituting the aqueous dispersion of the pseudopolyrotaxane after the production step.

### Claim 6 (depends on 1)

The method for producing the aqueous dispersion of the pseudopolyrotaxane according to claim 1,
wherein a temperature in mixing the polyethylene glycol and the cyclodextrin in the aqueous medium is from 50° C. to 100° C.

### Claim 7 (depends on 1)

The method according to claim 1, wherein the molecular cyclodextrin is α-cyclodextrin, β-cyclodextrin, or γ-cyclodextrin.

### Claim 8 (depends on 1)

The method according to claim 1, wherein the basic compound suppresses an increase in an inclusion amount of the cyclodextrin with time in the aqueous dispersion of the pseudopolyrotaxane.