# US 8,785,520 B2 · Process for production of polylactic acid resin composition

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- Number: US 8,785,520 B2
- Document ID: US8785520B2
- Status: Granted
- Kind: B2
- Application number: 13/522,648
- Filed: 2011-01-25
- Published: 2012-11-22
- Granted: 2014-07-22
- Earliest claimed: 2010-02-02
- Assignees: Kao Corporation
- Applicants: Tomoya Tsuboi; Akira Takenaka; Masahiro Mori
- Inventors: Tomoya Tsuboi; Akira Takenaka; Masahiro Mori
- Web page: https://patentgrep.com/patent/US8785520B2

## CPC

- B29B 7/007: {for continuous mixing}
- C08L 93/04: Rosin
- B29B 7/72: Measuring, controlling or regulating
- C08J 3/201: {Pre-melted polymers}
- C08K 5/0083: {Nucleating agents promoting the crystallisation of the polymer matrix}
- C08K 5/098: Metal salts of carboxylic acids
- C08K 5/20: Carboxylic acid amides
- C08K 5/42: Sulfonic acids; Derivatives thereof
- C08K 5/521: Esters of phosphoric acids, e.g. of H3PO4
- C08K 5/5317: Phosphonic compounds, e.g. R—P(:O)(OR')2
- C08K 9/04: Ingredients treated with organic substances {(treated with macromolecular compounds C08K9/08)}
- C08K 9/10: Encapsulated ingredients
- C08L 67/04: Polyesters derived from hydroxycarboxylic acids, e.g. lactones (C08L67/06 takes precedence)
- C08J 2367/04: Polyesters derived from hydroxy carboxylic acids, e.g. lactones (C08J2367/06 takes precedence)
- B29B: PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- C08L: COMPOSITIONS OF MACROMOLECULAR COMPOUNDS (compositions based on polymerisable monomers C08F, C08G; artificial filaments or fibres D01F; textile treating compositions D06)
- 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)
- C08K: Use of inorganic or non-macromolecular organic substances as compounding ingredients (paints, inks, varnishes, dyes, polishes, adhesives C09)

## Abstract

A method for producing a polylactic acid resin composition, including the following steps (1) and (2): step (1): subjecting an organic crystal nucleating agent to a wet pulverization in the presence of a carboxylic acid ester having a weight-average molecular weight of from 150 to 600 and a viscosity at 23° C. of from 1 to 500 mPa·s and/or a phosphoric ester having a weight-average molecular weight of from 150 to 600 and a viscosity at 23° C. of from 1 to 500 mPa·s to give a finely pulverized organic crystal nucleating agent composition; and step (2): melt-kneading a raw material for a polylactic acid resin composition comprising the finely pulverized organic crystal nucleating agent composition obtained in the step (1) and a polylactic acid resin.

## Claims

### Claim 1

A method for producing a polylactic acid resin composition, comprising the following steps (1) and (2):
step (1): subjecting an organic crystal nucleating agent to a wet pulverization in the presence of a phosphoric ester having a weight-average molecular weight of from 150 to 600 and a viscosity at 23° C. of from 1 to 500 mPa·s to give a finely pulverized organic crystal nucleating agent composition; and
step (2): melt-kneading a raw material for a polylactic acid resin composition comprising the finely pulverized organic crystal nucleating agent composition obtained in the step (1) and a polylactic acid resin.

### Claim 2 (depends on 1)

The method for producing a polylactic acid resin composition according to claim 1, wherein the organic crystal nucleating agent comprises at least one organic compound selected from the group consisting of metal salts of dialkyl aromatic sulfonates, metal salts of phosphoric esters, metal salts of phenylphosphonic acids, metal salts of rosin acids, aromatic carboxylic acid amides, and rosin acid amides.

### Claim 3 (depends on 1)

The method for producing a polylactic acid resin composition according to claim 1, wherein the organic crystal nucleating agent comprises a metal salt of a phenylphosphonic acid.

### Claim 4 (depends on 1)

The method for producing a polylactic acid resin composition according to claim 1, wherein the finely pulverized organic crystal nucleating agent composition has a volume-median particle size (D50) of from 50 to 700 nm.

### Claim 5 (depends on 1)

The method for producing a polylactic acid resin composition according to claim 1, wherein the step (1) comprises subjecting the organic crystal nucleating agent to a wet pulverization in the presence of the phosphoric ester, within a range satisfying a ratio of the weight of the organic crystal nucleating agent and a total weight of the phosphoric ester, that is the organic crystal nucleating agent/the phosphoric ester, of from 1/99 to 50/50.

### Claim 6 (depends on 1)

The method for producing a polylactic acid resin composition according to claim 1, wherein the phosphoric ester comprises a compound represented by the formula (I):
wherein each of R1, R2, and R3 is independently an alkyl group having from 1 to 4 carbon atoms; each of A1, A2, and A3 is independently an alkylene group having 2 or 3 carbon atoms; each of m, n, and p is independently a positive number representing an average number of moles added for the oxyalkylene group, wherein m+n+p is a number that exceeds 3 and is equal to or less than 12.

### Claim 7 (depends on 6)

The method for producing a polylactic acid resin composition according to claim 6, wherein m+n+p in the formula (I) is a number that exceeds 4 and is less than 12.

### Claim 8 (depends on 1)

The method for producing a polylactic acid resin composition according to claim 1, wherein the phosphoric ester is one or more members selected from the group consisting of tris(ethoxyethoxyethyl)phosphate, tris(methoxyethoxyethyl)phosphate, tris(propoxyethoxyethyl)phosphate, tris(butoxyethoxyethyl)phosphate, tris(methoxyethoxyethoxyethyl)phosphate, tris(ethoxyethoxyethoxyethyl)phosphate, bis(ethoxyethoxyethyl)methoxyethoxyethoxyethyl phosphate and bis(methoxyethoxyethoxyethyl)ethoxyethoxyethyl phosphate.

### Claim 9 (depends on 1)

The method for producing a polylactic acid resin composition according to claim 1, wherein the organic crystal nucleating agent subjected to the wet pulverization has a volume-median particle size (D50) of from 500 nm to 5 μm.

### Claim 10 (depends on 1)

The method for producing a polylactic acid resin composition according to claim 1, wherein the treatment temperature for the wet pulverization is from 5° to 250° C.

### Claim 11 (depends on 1)

The method for producing a polylactic acid resin composition according to claim 1, wherein the organic crystal nucleating agent is wet pulverized in step (1) with a media pulverizer.

### Claim 12 (depends on 1)

The method for producing a polylactic acid resin composition according to claim 1, wherein in the step (2) the finely pulverized organic crystal nucleating agent composition obtained in the step (1) is contained in an amount of from 1 to 50 parts by weight, based on 100 parts by weight of the polylactic acid resin.