# US 2014/0154937 A1 · Process for the production of a fiber-reinforced composite material

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- Number: US 2014/0154937 A1
- Document ID: US20140154937A1
- Status: Published application
- Kind: A1
- Application number: 14/095,324
- Filed: 2013-12-03
- Published: 2014-06-05
- Earliest claimed: 2012-12-04
- Assignees: BASF SE
- Applicants: BASF SE
- Inventors: Philippe Desbois; Silke Biedasek
- Web page: https://patentgrep.com/patent/US20140154937A1

## CPC

- D06N 3/125: {with polyamides}
- C08J 5/04: Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J 5/043: {with glass fibres}
- C08J 5/243: {using carbon fibres}
- C08J 5/244: {using glass fibres}
- C08J 5/249: {characterised by the additives used in the prepolymer mixture}
- C08J 2377/02: Polyamides derived from omega-amino carboxylic acids or from lactams thereof (C08J2377/10 takes precedence)
- Y10T 428/2933: Coated or with bond, impregnation or core
- Y10T 442/198: Coated or impregnated
- Y10T 442/20: Coated or impregnated woven, knit, or nonwoven fabric which is not [a] associated with another preformed layer or fiber layer or, [b] with respect to woven and knit, characterized, respectively, by a particular or differential weave or knit, wherein the coating or impregnation is neither a foamed material nor a free metal or alloy layer
- D06N: WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- 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)
- Y10T: TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION

## Abstract

The present invention relates to a process for the production of a fiber-reinforced composite material with a polyamide matrix.

## Claims

### Claim 1

A process for producing a fiber-reinforced composite material with a polyamide matrix by
a) providing a solid polymerizable composition which comprises
A) at least one lactam,
B) at least one catalyst, and
C) at least one activator selected from isocyanates, anhydrides, acyl halides, reaction products of these with A), and mixtures of these,
b) applying, in solid, free-flowing form, the polymerizable composition provided in step a) onto a fiber material,
c) subjecting the fiber material obtained in step b) with the applied polymerizable composition to treatment at elevated pressure and at a temperature at which the mixture of components A), B), and C) is flowable, where this encloses and penetrates the fiber material,
d) cooling the product obtained in step c).

### Claim 2 (depends on 1)

The process according to claim 1, in which, in addition,
e) the product obtained in step d) is subjected to specific mechanical processes.

### Claim 3 (depends on 1)

The process according to claim 1, in which, in addition,
f) the product obtained in step d) is subjected to a forming process.

### Claim 4 (depends on 1)

The process according to claim 1, where the polymerizable composition provided in step a) comprises
from 50 to 99.7 parts by weight of at least one lactam A),
from 0.2 to 8.0 parts by weight of at least one catalyst B), and
from 0.1 to 3.6 parts by weight of at least one activator C),
based on the total weight of the composition.

### Claim 5 (depends on 1)

The process according to claim 1, where the polymerizable composition provided in step a) comprises at least one lactam A) selected from ε-caprolactam, 2-piperidone, 2-pyrrolidone, caprylolactam, enantholactam, laurylolactam, laurolactam, and mixtures of these.

### Claim 6 (depends on 1)

The process according to claim 1, where the polymerizable composition provided in step a) comprises at least one catalyst B) selected from sodium caprolactamate, potassium caprolactamate, magnesium bromide caprolactamate, magnesium chloride caprolactamate, magnesium biscaprolactamate, sodium hydride, sodium, sodium hydroxide, sodium methanolate, sodium ethanolate, sodium propanolate, sodium butanolate, potassium hydride, potassium, potassium hydroxide, potassium methanolate, potassium ethanolate, potassium propanolate, potassium butanolate, and mixtures of these.

### Claim 7 (depends on 1)

The process according to claim 1, where the polymerizable composition provided in step a) comprises at least one activator C) selected from hexamethyl diisocyanate, isophorone diisocyanate, hexamethylenedioyl bromide, hexamethylenedioyl chloride, and mixtures of these.

### Claim 8 (depends on 1)

The process according to claim 1, where the polymerizable composition provided in step a) is composed only of components A), B), and C).

### Claim 9 (depends on 1)

The process according to claim 1, where the polymerizable composition provided in step a) takes the form of particles with an average diameter in the range from 1 to 2000 μm.

### Claim 10 (depends on 1)

The process according to claim 1, where in order to provide the polymerizable composition in step a) components A), B), and C) are combined in liquid form at elevated temperature, the combined components are mixed, and then the mixture is hardened by cooling.

### Claim 11 (depends on 10)

The process according to claim 10, where the time from formation of the combined mixture of components A), B), and C) to hardening is from 1 millisecond to 10 minutes.

### Claim 12 (depends on 10)

The process according to claim 10, where the temperature of the combined mixture of components A), B), and C) is at most 20° C. above the melting point of said mixture.

### Claim 13 (depends on 10)

The process according to claim 10, where in order to provide the polymerizable composition in step a)
components A), B), and C) are separately melted and combined, or
a first melt made of the catalyst B) and of at least one lactam A), a second melt made of the activator C) and of at least one lactam A), and optionally, in addition, a third melt made of at least one lactam A) are combined,
the combined components are mixed, and then the mixture is hardened by cooling.

### Claim 14 (depends on 1)

The process according to claim 1, where the provision of the polymerizable composition in step a) comprises the following steps:
a1) mixing of components A), B), and C) at a temperature which is the same as or higher than the melting point of a mixture composed only of components A), B), and C),
a2) conversion of the mixture into droplet form,
a3) cooling of the droplets obtained in step a2) to a temperature at least 10° C. below the melting point of the mixture;
a4) optionally granulation of the cooled mixture.

### Claim 15 (depends on 1)

The process according to claim 1, where the fiber material used in step b) comprises continuous-filament fibers, or is composed of continuous-filament fibers.

### Claim 16 (depends on 1)

The process according to claim 1, where the fiber material used in step b) is one selected from fiber bundles, woven fabrics, knitted fabrics, laid scrims, or nonwovens, in each case made of continuous-filament fibers.

### Claim 17 (depends on 1)

The process according to claim 1, where the treatment in step c) takes place under conditions under which the lactam A) in essence polymerizes to completion.

### Claim 18 (depends on 17)

The process according to claim 17, where the temperature in step c) is in the range from 80 to 250° C.

### Claim 19 (depends on 17)

The process according to claim 17, where the product obtained in step c) has at most 5% by weight residual content of lactam A), based on the weight of the lactam A) in the polymerizable composition used in step a).

### Claim 20 (depends on 1)

The process according to claim 1, where the treatment in step c) takes place under conditions under which the lactam A) does not in essence polymerize to completion.

### Claim 21 (depends on 20)

The process according to claim 20, where the treatment in step c) takes place at a temperature of from 1 to 20° C. above the melting point of the mixture of components A), B), and C).

### Claim 22 (depends on 20)

The process according to claim 20, where the product obtained in step c) has at most 50% by weight content of polymeric components, based on the total weight of the polymerizable compounds in the solid polymerizable composition used in step a).

### Claim 23 (depends on 1)

The process according to claim 1, where the pressure during treatment in step c) is in the range from 5 to 300 bar.

### Claim 24 (depends on 1)

A fiber-reinforced composite material obtainable via a process according to claim 1.

### Claim 25 (depends on 24)

The fiber-reinforced composite material according to claim 24, which has content of fibers and fillers in the range from 30 to 90% by weight, based on the total weight of the fiber-reinforced composite material.

### Claim 26 (depends on 2)

The process according to claim 2, in which, in addition,
f) the product obtained in step e) after specific mechanical processes is subjected to a forming process.