Method for producing pseudopolyrotaxane

Patent metadata

Field	Value
Publication number	US-9938382-B2
Application number	US-201113994515-A
Country	US
Kind code	B2
Filing date	Dec 5, 2011
Priority date	Dec 16, 2010
Publication date	Apr 10, 2018
Grant date	Apr 10, 2018

Abstract

The present invention aims to provide an industrially advantageous method of producing a powdery pseudopolyrotaxane with a high inclusion ratio. The present invention relates to a method for producing a pseudopolyrotaxane, including: an inclusion step of mixing a polyethylene glycol and a cyclodextrin in an aqueous medium to form an aqueous dispersion of pseudopolyrotaxane that contains pseudopolyrotaxane particles in which the polyethylene glycol is included in the cavities of the cyclodextrin molecules in a skewered manner; and a drying step of drying the aqueous dispersion of pseudopolyrotaxane produced in the inclusion step to obtain the pseudopolyrotaxane. In the drying step, the aqueous dispersion of pseudopolyrotaxane is sprayed and dried in a heated gas-stream.

First claim

The invention claimed is:

1. A method for producing a pseudopolyrotaxane, comprising:
an inclusion step of mixing polyethylene glycol and cyclodextrin in an aqueous medium so as to form an aqueous dispersion of pseudopolyrotaxane, which comprises pseudopolyrotaxane particles in which the polyethylene glycol is included in cavities of molecules of the cyclodextrin in a skewered manner; and
a drying step of drying the aqueous dispersion of the pseudopolyrotaxane produced in the inclusion step so as to obtain the pseudopolyrotaxane in a dry form,
wherein, in the inclusion step, the polyethylene glycol and the cyclodextrin are dissolved in the aqueous medium so as to form a mixed solution, and the mixed solution is continuously or intermittently cooled at a cooling speed in a range from 0.05 to 30° C./min. while the mixed solution flows without being left to stand by stirring at a rotational speed between 75 and 7000 rpm, so that the pseudopolyrotaxane particles form, and thereby the aqueous dispersion of the pseudopolyrotaxane is produced, and
wherein a weight ratio between the polyethylene glycol and the cyclodextrin is in a range from 1:3 to 1:5,
wherein the pseudopolyrotaxane particles in the aqueous dispersion of the pseudopolyrotaxane have a volume average particle size in a range from 1 to 50 μm, and
wherein, in the drying step, the aqueous dispersion of the pseudopolyrotaxane is sprayed by a nozzle method and dried in a heated gas-stream.

2. The method for producing the pseudopolyrotaxane according to claim 1 ,
wherein the polyethylene glycol has a weight average molecular weight in a range from 1,000 to 500,000.

3. The method for producing the pseudopolyrotaxane according to claim 1 ,
wherein a solid concentration of the aqueous dispersion of pseudopolyrotaxane is in a range from 5 to 25% by weight.

4. The method for producing the pseudopolyrotaxane according to claim 1 ,
wherein a gas-stream temperature in the drying step is in a range from 70 to 200° C.

5. The method for producing the pseudopolyrotaxane according to claim 1 ,
wherein pressure in a system in the drying step is equal to or lower than the atmospheric pressure.

6. The method for producing the pseudopolyrotaxane according to claim 1 ,
wherein the flowing of the mixed solution is performed by flowing continuously the mixed solution by at least one method selected from the group consisting of stirring with a blade and homogenizing.

7. The method for producing the pseudopolyrotaxane according to claim 1 ,
wherein the drying step is carried out in a spray dryer with an inlet temperature between 120 and 188° C. and an outlet temperature between 70 and 90° C.

Assignees

• Yamasaki Tomoaki
• Okazaki Shinya
• Okazaki Hiroki
• Hamamoto Shigeki
• Zhao Changming
• Sumitomo Seika Chemicals
• Advanced Softmaterials Inc

Inventors

• Yamasaki Tomoaki
• Okazaki Shinya
• Okazaki Hiroki
• Hamamoto Shigeki
• Zhao Changming

Classifications

• C08J3/12 Primary

  Powdering or granulating · CPC title

• C08J2371/02

  Polyalkylene oxides · CPC title

• C08B37/0015

  Inclusion compounds, i.e. host-guest compounds, e.g. polyrotaxanes · CPC title

• C08G83/007 Primary

  Polyrotaxanes; Polycatenanes · CPC title

• C08L5/16

  Cyclodextrin; Derivatives thereof · CPC title