# US 7,745,504 B2 · Process for producing porous spherical polyamide particle

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- Number: US 7,745,504 B2
- Document ID: US7745504B2
- Status: Granted
- Kind: B2
- Application number: 11/883,503
- Filed: 2006-02-02
- Published: 2008-07-03
- Granted: 2010-06-29
- Earliest claimed: 2005-02-02
- Assignees: Ube Industries, Ltd.
- Inventors: Kimio Nakayama; Tatsuya Shoji; Yukihiko Asano; Shigeru Yao
- Web page: https://patentgrep.com/patent/US7745504B2

## CPC

- C08J 9/28: by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
- C08J 3/14: by precipitation from solutions {(C08J3/122 takes precedence)}
- C08J 2201/0543: the non-solvent being organic
- C08J 2201/0546: the non-solvent being organic
- C08J 2377/00: Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J 2377/02: Polyamides derived from omega-amino carboxylic acids or from lactams thereof (C08J2377/10 takes precedence)
- 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)

## Abstract

Porous spherical particles of polyamide 11 or polyamide 12 can be produced by an industrially advantageous process which comprises the steps of mixing a polyamide solution of polyamide 11 or polyamide 12 dissolved in a phenol compound and a low molecular weight aliphatic alcohol which is a poor solvent for the polyamides but is well compatible with the phenol compound in the presence of a high molecular weight alkylene glycol to prepare a mixture solution having an initial viscosity of 10 mPa·s or more, and allowing the mixture solution to stand, to precipitate polyamide particles.

## Claims

### Claim 1

A process for producing porous polyamide particles which comprises the steps of mixing a polyamide solution of polyamide 11 or polyamide 12 dissolved in a phenol compound and a low molecular weight aliphatic alcohol which is a poor solvent for the polyamides but is compatible with the phenol compound in the presence of a high molecular weight alkylene glycol to prepare a mixture solution having an initial viscosity of 10 mPa·s or more, and allowing the mixture solution to stand, to precipitate the polyamide particles.

### Claim 2 (depends on 1)

The process of claim 1, wherein the mixture solution is prepared by mixing the polyamide solution containing the high molecular weight alkylene glycol with the low molecular weight aliphatic alcohol.

### Claim 3 (depends on 1)

The process of claim 1, wherein the mixture solution is prepared by mixing the polyamide solution with the low molecular weight aliphatic alcohol containing the high molecular weight alkylene glycol.

### Claim 4 (depends on 1)

The process of claim 1, wherein the mixture solution is prepared by simultaneously mixing the polyamide solution, the low molecular weight aliphatic alcohol, and the high molecular weight alkylene glycol.

### Claim 5 (depends on 1)

The process of claim 1, wherein the mixture solution is prepared by mixing the polyamide solution and the low molecular weight aliphatic alcohol, and then mixing the high molecular weight alkylene glycol.

### Claim 6 (depends on 1)

The process of claim 1, wherein the mixture solution is prepared to have a polyamide concentration in the range of 0.05 to 20 wt. %.

### Claim 7 (depends on 1)

The process of claim 1, wherein the mixture solution is prepared to have a high molecular weight alkylene glycol concentration in the range of 0.5 to 10 wt. %.

### Claim 8 (depends on 1)

The process of claim 1, wherein the phenol compound is phenol.

### Claim 9 (depends on 1)

The process of claim 1, wherein the low molecular weight aliphatic alcohol is a mixture of a trihydric alcohol and a low molecular weight alkylene glycol or a mixture of a trihydric alcohol and a monohydric alcohol.

### Claim 10 (depends on 9)

The process of claim 9, wherein the trihydric alcohol is glycerol.

### Claim 11 (depends on 1)

The process of claim 1, wherein the low molecular weight aliphatic alcohol is a mixture of glycerol and ethylene glycol.

### Claim 12 (depends on 1)

The process of claim 1, wherein the low molecular weight aliphatic alcohol is a mixture of glycerol and a monohydric alcohol having 1 to 6 carbon atoms.

### Claim 13 (depends on 1)

The process of claim 1, wherein the high molecular weight alkylene glycol is polyethylene glycol having a number average molecular weight of 1,000 or more, polypropylene glycol having a number average molecular weight of 1,000 or more, or a mixture thereof.

### Claim 14 (depends on 1)

The process of claim 1, wherein the initial viscosity of the mixture solution is not higher than 200 Pa·s.

### Claim 15 (depends on 1)

The process of claim 1, wherein the step of allowing the mixture solution to stand is performed for at least 30 minutes.

### Claim 16 (depends on 1)

The process of claim 1, wherein the step of allowing the mixture solution to stand is performed at a temperature in the range of 20 to 80° C.